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Nanospray Users Guide - Agilent Technologies

1. MS Workstation Parameter Starting Value Application Trap Column Equilibration Flow Rate 5 uL min Method Trap Column Equilibration Volume 15 uL Method Analytical Column Equilibration Flow Rate 300 600 nL min Method Analytical Column Equilibration Volume 2 uL Method Sample Pickup Flow Rate 10 pL min unless sample is viscous Sample List Sample Pickup Volume Volume injected onto the column Sample List Sample Loading Flow Rate Use trap equilibration flow Sample List Sample Loading Volume 10 pL 1 5 times sample volume Sample List T These parameters depend on the column or trap 17 Optimizing the Drying Gas Flow Rate Drying gas flow rate and temperature influence ion generation e Mobile phases with a high percentage of organic usually have high vapor pressures These mobile phases need low drying gas temperatures typically 150 C for 300 nL min infusions e Highly aqueous solvent compositions need high drying gas temperatures typically 200 300 C if the water is 85 at flow rates of 280 30 mL min e The actual drying gas flow needed is dependent upon the nature of the analytes If the temperature is too high the analyte can precipitate in the emitter tip Optimizing the Spray for a Gradient To maintain optimum spray conditions throughout a gradient run the drying gas temperature and the emitter voltage can be ramped during runs Use isocratic conditions to determine the optimum settings
2. Limitaciones de recursos y responsabilidades Los recursos provistos en lo citado son nica y exclusivamente los del cliente Varian no podr ser responsable en ning n caso por dafios imprevistos o consecuencias p rdida de uso p rdida de producci n o cualquier otra p rdida incurrida 1 of 1 Operating Instructions Safety Information This instruction manual is provided to help you establish operating conditions which will permit safe and efficient use of your equipment Special considerations and precautions are also described in the manual which appear in the form of NOTES CAUTIONS and WARNINGS as described below It is important that you operate your equipment in accordance with this instruction manual and any additional information which may be provided by Varian Address any questions regarding the safe and proper use of your equipment to your local Varian office NOTE Information to aid you in obtaining optimal performance from your instrument Warning Symbol WARNING SHOCK HAZARD WARNING CHEMICAL HAZARD WARNING BURN HAZARD A WARNING EYE HAZARD AN WARNING FIRE HAZARD 2 WARNING ZA EXPLOSION HAZARD WARNING RADIATION SOURCE AN WARNING MOVING PARTS 03 914603 00 11 CAUTION Alerts you to situations that may cause moderate injury and or equipment damage and how to avoid these situations Warning Description WARNING Alerts you to potentially hazardous situations that cou
3. www varianinc com 03 914603 84 11 Contents Overview OF APC ai 3 INIFOGUGHON pL 3 Basic Pfinciples REDDE 3 Positive lom APCI vt LE 4 Negative lon APG PEE 4 Pesce 5 Installation ot APCI Chamber eed A esae i 6 APCI Daily Startup and Shutdown iii 8 SO eee ERE eed en LE a eae A eae Gen 8 Wes 8 TUNING 8 APCI Mobile Phase Selectioti a oie tette della RB RE E nex kane da 8 Optimizing S N for APE iet eet meten tete Da fare Meat it Erin e be ca dia 9 Typical APGI Operating Parameters a reete ee ee reete til niet nl cad 9 APGI Performance Evaluation trece rales even 10 Operating Conditions for Testing the APCI arrancar 10 ARG SENSIIVIY Testi er alta 10 APCI General Maintenance 2 aer rera prre can se ceu ix kr re duas Due Dra Ra du 11 Cleaning sito dero t ete n Eft hri d e i iei Ie ette LEE LA at 11 Cleaning the Spray Shield iih ette i ded oed ete ot e thee 11 Cleaning the Vacuum Gapillaty cotidiana 11 Cleaning the Corona Needl 5 m tied adh tec et iae die tote dti ee DO eH etie eae 12 Replacing and Aligning the Corona Needle iii 12 Replacing the Nebulizing Needle iii 13 hemovalsii stretti ed eet e te det A de cd tee dne I RAS RER EE 13 Installations oio daten t free eet fce edt tet cere E ee hilf 13 Replacing the APGI Quartz Tube ae ra el 13 Re moving th Quartz Tubertin
4. Abschirmung die das Bedienungspersonal gegen Abstrahlungen sch tzt Zum st ndigen Schutz m Achten Sie darauf da die sch tzende Lampenab deckung der Detektoren mit variablen und festen Wellenl ngen w hrend des Betriebs an ihrem Platz ist m Schauen Sie nicht direkt in die Fl ssigkeitszellen im Detektor oder in die UV Lampe Zum In spizieren der Lichtquelle oder der Fl ssigkeitszelle benutzen Sie immer einen wirksamen Augenschutz wie er durch Borsilikatglas oder Polystyrol gew hr leistet wird 3 of 4 Verf gbarkeit von Ersatzteilen Es ist Varian s Grundsatz Ersatzteile f r alle Instrumente und die wichtig sten Zubeh re f r einen Zeitraum von f nf 5 Jahren nach dem Fertigung sauslauf dieser Ger teserie verf gbar zu haben Nach diesem Zeitraum von f nf 5 Jahren k nnen Ersatzteile auf der Basis solange vorhanden be zogen werden Als Ersatzteil werden hier solche elektrischen und mecha nischen Einzelteile verstanden die unter normalen Bedingungen ausfallen k nnen Beispiele sind Relais Lampen Temperaturf hler Detektorele mente Motore usw Metallbleche Formteile oder Baugruppen und GuBteile PC Boards und Funktionsmodule k nnen normalerweise neu wert hnlich f r eine brauchbare Lebensdauer instandgesetzt werden und werden deshalb nur auf der Basis solange vorhanden nach dem Produk Serviceverf gbarkeit Varian bietet seinen Kunden auch nach dem Auslaufen der Garantie eine Vielfalt von Servicel
5. Transferleitungen flexible Disketten Magnetbandkasset ten elektronische Vervielfacher Hitzdr hte Vakuum Gaskets Sitzfl chen und alle Teile die den Proben und mobilen Phasen ausgesetzt sind Diese Garantie erlischt bei eingetretenem Unfall fal scher Benutzung Umbau Mi brauch Vernachl s sigung Bruch falscher Benutzung oder falscher War tung unbefugten oder falschen Modifikationen oder Basteleien Benutzung in ungeeigneter physikalischer Umgebung Benutzung mit marginaler Stromversorgung oder Benutzung mit anderen ungen genden Einrichtun gen oder Versorgungen Mit vern nftiger Sorgfalt m ssen Gefahren vermieden werden Diese Garantie steht ausdr cklich anstelle von allen anderen angedeuteten Garantien und schlie t sie aus einschlie lich aber nicht beschr nkt auf Garan tien der Verk uflichkeit und Eignung f r einen be sonderen Zweck Gebrauch oder Anwendung und allen anderen Verpflichtungen oder Haftungen von Varian s Seite wenn nicht solche Garantien Verpflichtungen oder Haftungen ausdr cklich schriftlich mit Varian vereinbart wurden Beschr nkung der Hilfen und Haftung Die hier gegebenen Hilfen sind einzig und allein Sa che des Kunden In keinem Fall wird Varian f r versehentliche oder sich ergebende Sch den wie Nutzungsverlust Produktionsverlust oder jeden an deren Verlust haften 1 von 1 dy AS VARIAN Systemes de qualit chez Varian Inc Les normes ISO s rie 9000 ont t cr
6. es Gen ve en 1987 pour rem dier la confusion dans la d finition des normes de qualit Ces normes d finissent un mod le de contr le de qualit dans le domaine de la conception produit du d veloppement de la production des installations des services et du support client Elles constituent pr sent la r f rence mondiale en mati re de contr le de qualit utilis e aux fins d valuation du niveau d engagement d une entreprise dans ce domaine et la valeur de ses syst mes de qualit Plusieurs organisations de par le monde telle la British Standards Institution BSI offrent les services d auditeurs qualifi s et objectifs charg s d examiner les proc dures de qualit le d veloppement de produit les proc d s de fabrication et les programmes de satisfaction du client Aucune soci t ne peut se pr valoir de l homologation ISO 9000 sans avoir re u l approbation des valuateurs rigoureux de la BSI ou d un organisme accr ditif similaire L homologation ISO 9000 constitue une valuation objective d un tiers afin de d terminer le niveau d engagement d un fournisseur dans le domaine de la qualit En 1992 Varian Analytical Instruments a re u l homologation ISO 9001 normes des plus compl tes de la s rie ISO 9000 En d autres termes chaque tape du processus de qualit notamment le d veloppement produit la fabrication le test final l exp dition et les fournitures de pi ces a t s oumis un contr le
7. n ha sido pagada por el cliente o incluida en el precio de compra el plazo de garant a comenzar a partir de la fecha de conclusi n de la instalaci n Si el cliente especifica que la instalaci n comenzar 30 d as despu s 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 preinstalaci n de Varian o cualquier otra omisi n por parte del cliente el plazo de garant a comenzar el trig simoprimer d a a partir del env o Adem s Varian cobrar al cliente por trabajos y otros gastos relacionados con intervenciones de servicio de instalaci n m ltiples o tard as Productos de software Cuando el software se suministra dentro del marco de una licencia de utilizaci n acordada entre Varian y el cliente cualquier garant a estar estrictamente limitada a los t rminos del citado acuerdo En ausencia de una licencia de utilizaci n y a no ser que exista un acuerdo de per odo de garant a por escrito entre Varian y el cliente el per odo de garant a ser el fijado de acuerdo con los t rminos 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 seg n lo descrito en Manual de instrucciones y que est libre de defectos que impidan la ejecuci n de instrucciones de programaci n Sin embargo Va
8. situada durante su funcionamiento m No mire directamente a las celdas del detector 6 a la fuente de luz UV Cuando inspeccione la fuente de luz la celda utilice siempre una protecci n para los ojos como gafas de borosilicato 6 poliestireno 3 of 4 Disponibilidad de Recambios Es Pol tica de Varian disponer de Recambios para cualquier instrumento y la mayor a de los accesorios por un periodo de cinco 5 a os despu s del ltimo instrumento fabricado Los recambios durante esos cinco a os estar n disponibles pero siempre bajo el sistema Seg n disponibilidad Los Recambios est n definidos como todas aquellas partes individuales 2 mec nicas 6 el ctricas que son susceptibles de fallo durante su normal proceso de operaci n Por ejemplo rel s l mparas sondas de temperatura elementos del detector motores etc Las planchas de metal partes de la estructura placas de circuitos integrados y otros m dulos funcionales son normalmente susceptibles de reparaci n y por lo tanto s lo estar n disponibles bajos el sistema Seg n disponibilidad despu s del ltimo instrumento fabricado Oficinas de Instrumentaci n Anal tica Varian Para cualquier consulta sobre Instrumentaci n Anal tica Servicio T cnico 6 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 V sendorf bei Wien Tel 43
9. 1 699 9669 Benelux Bergen Op Zoom Tel 31 164 282 800 Brazil and Latin America S S o 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 4 of 4 France Les Ulis C dex 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 Disponibilidad de Servicio Varian ofrece una gran variedad de sistemas de Servicio para mantener el soporte a sus usuarios tras el periodo de garantfa El Soporte de Servicio se ofrece a trav s de atractivos Contratos de Servicio 6 bajo un sistema de facturaci n de mano de obra y materiales El mantenimiento y el entrenamiento se realiza por ingenieros cualificados bajo Contrato 6 petici n United States Walnut Creek California USA Tel 1 800 926 3000 GC and GC MS Tel 1 800 367 4752 LC Ar A VARIAN
10. All brand and product names are trademarks or registered trademarks of their respective owners Contents Introduction EEE UM LE 3 ONE 3 Offline Analysis cuisine demie 3 MISI 4 BASTE Operation QR PN 5 OVOI VIOW sia fies en ee e Eo e eoe e te dii tet A tete Deo evel ed d nd Be PL cab rege 5 Inst lling the ESI lon Source Leben i dd beo dte ueste ed ntl que 7 Installing the nES lon Source siii tu A dete densae 7 Installing and Operating the Camera siennes 8 Installing the Gamera SOftware tue det ice cute de cine ciet rt dee 8 Connecting the Camera 3 tein Tatio p A tede etus 8 Setting Up the Camera Software pa ne eR eR ed et e edidi 8 Installing an Online Emitter for Infusion Analysis eee ee tenets erent ee eeeaeeeeeeaeeeeeeaeeeesenaeeeesenaeeeeeeaas 8 Assembling the Syringe and Emitter 1 ei HR dedero areale 9 Assembling an Online Emitter 2 2 rie aa 10 Positioning the Gatmera ii peni Ee dial eed a 11 Positioning an Online Emitter atico tede eee ho e Pe eed tus 12 Setting Workstation Parameters and Optimizing Emitter Conditions 13 Parameters for the nESI lon Source ene nennen meer enne nennen nennen nennen nnne 14 Operatia PME sea ea a b et gd c eed tette Med n pineale 14 Using a Column and Nanoflow LC is E a irit nene inneren nennen nennen 15 OVEIVIEW Aid buo adele asa tec tetuer dt
11. 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 trac
12. Resuts Format Chromategram Format Compound Reports Calbraton Bleck Repert Format Summary Report Format Recuks Troatmont Method Segrent Detector On Scan Type Ful z ScanMode Standes Data F I Syirge Pump On General Parameters Ionization Control Nanosprey lonization Parameters Ful Scan Parameters T Emitte Vokage Positive vote Negabve H volts D Dying Gas Presume pa T Spray ShildVolags F DryingGas Temperate 52 C Positive vote Negative Sj vote Figure 17 Emitter Voltage Ramp The emitter voltage or can be ramped over the course of an entire run similar to the Drying Gas and Vaporizer Gas Temperature Ramps for ESI and APCI applications In nESI a Drying Gas Temperature Ramp can be set in addition to the Emitter Voltage Ramp To set the emitter voltage or drying gas temperature ramp Click Use Ramp Rate to enable it Enter an Initial Hold Time if needed Enter the Start Emitter Voltage or Start Temperature Enter the Ramp End Time gr Ns A Enter the End Emitter Voltage or End Temperature The Emitter Voltage or Temperature at Method End and Ramp Rate are automatically determined from the entered values 26 Nanospray lonization Setpoints Figure 18 27 28 216 LC Pump Configuring the 216 LC with MS Workstation Configuring the 216 LC for MS Workstation Control 1 Using the appropriate Start In Sync Cable provided with your 216 LC System
13. Sample Loading A 48 6 210 4 bar B 0 1 0 0 bar Run Gradient A 77 9 163 3 bar B 87 6 173 5 bar This dialog box documents software and hardware information It also captures the pressure ranges for the key stages of the last cycle Similar info is saved in the GLP log included in each data file 37 216 LC SampleList Window Extensions When MS Workstation controls a 216 LC the SampleList has the following fields Refer to the generic SampleList Window help for a description of the fields not listed here Sample Name Mill Sample Type Cal Injection A level Ini Notes AutoLink Item Pickup Vol uL Pickup Flow uL min Loading Vol uL Loading Flow uL min Vial Pickup Pickup Flow Loading Loading Flow Amount Std Vol uL fuL min Vol uL ul min IS N only Add Fill Down Add Lines Defaults Description Amount of sample to be picked up 0 1 18 0 uL Flow rate of the S pump during sample pickup 0 01 40 0 uL min Volume to be loaded onto the trap column 0 0 137 0 uL Flow rate of Pump A while sample is being loaded onto the trap column 0 01 100 0 uL min Hardware Dialog Box 216 LC AutoSampler Hardware Loop Volume uL 250 Cancel Plate Type 446 24 2mL vials y 4x6 24 2mL vials 8x12 96 well plate 16x24 384 well plate Item Loop Volume uL Plate Type Description Volume of Sample Loop
14. are fragile The manufacturers of offline tips provide detailed information and recommendations on their web sites 48
15. assembly Luer Syringe Fingertight Nut UCF 33001 Adapter UCP 659 e To Emitter Adapter Ferrule UCF151 Fused Silica Tubing UCFS150 or PEEK Tubing UC1579L 100 uL Syringe HM 81020 Figure 4 3 Putthe syringe on the syringe drive NOTE All connections must be bottomed out and tubing must be flush with sleeves Assembling an Online Emitter 1 Step 1 Column or fused silica from infusion source with a sleeve Ferrule Connect the union to the column or to the fused silica tubing from the syringe Carefully remove the emitter from the package Do not bend it Check that the emitter is flush with the end of the sleeve To ensure that the emitter stays flush with the sleeve handle the sleeve not the emitter during the following steps Insert the sleeve end of the emitter into the nut then into the ferrule making sure the sleeve and emitter extend through the ferrule a few millimeters To minimize the connection volume the sleeve must be bottomed out in the union when the nut is tightened Insert the ferrule into the conductive union Tighten the nut connector firmly while gently pressing the sleeve to ensure that it is bottomed out in the union Emitter Adapter Sleeve Nut Ferrule yo Housing D Insert e Conductive Union for 1 32 in tubing UCUH432 Stainless Steel Emitter 393275209 Figure 5 Install the conductive union into the clamp on the nanospray interface and
16. 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 1 of 1 ap A VARIAN Qualitatssysteme bei Varian Inc Die Standards der ISO 9000 Serien wurden 1987 in Genf mit dem Ziel geschaffen das Durch einander gegens tzlich
17. cette situation Description Symboles d avertissement AN R MM c a D ELECTROCUTION ATTENTION SUBSTANCES CHIMIQUES DANGER ATTENTION RISQUE DE BRULURES A ATTENTION DANGER POUR LES YEUX ATTENTION RISQUE D INCENDIE A ATTENTION ZA RISQUE D EXPLOSION ATTENTION SOURCE DE RADIATION ATTENTION PIECES EN MOUVEMENT 03 914603 82 11 Exposition des tensions dangereuses D brancher le mat riel du secteur avant de d visser les panneaux protecteurs Pr sence ventuelle de substances chimiques dangereuses Eviter tout contact en particulier lors du remplissage des r servoirs Prendre les mesures de protection ad quates pour les yeux et la peau Exposition des surfaces chaudes ou trait es cryog niquement Prendre les mesures de protection ad quates pour la peau Les dommages caus es aux yeux sont de deux natures diff rentes jet de particules et de produits chimiques ou radiations UV Utiliser des protections du visage et des yeux appropri es Risque potentiel d incendie Se conformer aux instructions du manuel pour faire fonctionner le mat riel en toute s curit Risque potentiel d explosion en raison du type de gaz ou de liquide utilis Pr sence d une source de radiation ionisante Se conformer aux instructions du manuel pour faire fonctionner le mat riel en toute s curit Garder les mains et les doigts hors de port e Ar as VARIAN 10f4 Pr cautions g n rales en mati re de s
18. che sono sostanzialmente esenti da difetti che impediscano l esecuzione delle rispettive istruzioni di programma La Varian non garantisce alcun funzionamento ininterrotto o senza errori Interventi Tecnici Gli unici interventi previsti dalla garanzia sull hardware sono o la riparazione dei malfunzionamenti dello strumento che a giudizio della Varian siano dovuti o riconducibili a difetti di costruzione dei materiali originali o a discrezione della Varian la sostituzione dei componenti difettosi fermo restando che la Varian potr in alternativa optare per il rimborso di una congrua parte del prezzo d acquisto dello strumento o dell accessorio difettosi La riparazione o la sostituzione in garanzia non valgono a prorogare in alcun modo il periodo di garanzia originariamente previsto 03 914412 83 2 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 sar responsabile di eventuali danni o perdite subiti durante il trasporto dallo strumento o dall accessorio reso e dovr pagare le spese di spedizione in via anticipata La Varian restituir 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
19. con fusibles del tipo y tama o estipulados en el panel de fusibles en el manual Sustituya los cables deteriorados inmediatamente con cables del mismo tipo y graduaci n Asegureses de que los valores de las l neas de electricidad se ajustan a los valores para los que el Instrumento ha sido preparado Botellas de Gas Comprimido 2 of 4 Guarde y maneje las botellas de gas con cuidado y de acuerdo con las normas de seguridad Asegure las botellas a una estructura inmovil 6 a la pared Guarde y mueva las botellas en posici n vertical Retire los reguladores antes de transportarlas Guarde las botellas en un rea 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 s lamente reguladores y conexiones aprobadas Utilice s lo tubos de conexi n cromatogr ficamente l mpios Varian p n 03 918326 00 y que tengan una graduaci n de presi n significativamente mayor que la mayor presi n del regulador 03 914603 84 11 GC Pr cticas de Seguridad Sistema de Extracci n No se necesita un sistema de extracci n para los detectores GC instalados en un laboratorio bien ventilado excepto cuando se analicen muestras qu micas peligrosas Si instala un sistema de extracci n m Utilice conductos a prueba de fuego m Instale un ventilador al final del sistema m Instale entradas de aire cuya vi
20. e Reserpine Set the capillary between 80 to 120V and monitor m z 609 3 e 4 nitrophenol Set the capillary between 45 to 65V and monitor m z 138 0 e Injection 5 uL of either the reserpine or 4 nitrophenol solution which is 2 pg uL 10 pg injected APCI Sensitivity Test Positive APCI Set the SIM scan mode to mass 609 8 A signal to noise of approximately 20 1 RMS or greater should be attained for 10 pg uL reserpine 2 pg uL 5 uL injection by FIA at 1 mL min The mobile phase is 50 50 methanol water Check the results in Chro using 3 point smoothing Right click the peak to display the signal to noise ratio Negative APCI Set the SIM scan mode to mass 138 A signal to noise of approximately 20 1 RMS or greater should be attained for 10 pg uL nitrophenol 2 pg uL 5 uL injection by FIA at 1 mL min The mobile phase is 50 50 methanol water Check the results in Chro using 3 point smoothing Right click the peak to display the signal to noise ratio 10 03 914981 00 3 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 WARNING Materials used for cleaning can produce hazardous CHEMICAL H AZARD vapors Take appropriate precautions before beginning any cleaning procedure More extensive cleaning is required when se
21. 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 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 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 addebiter 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 purch regolarmente utilizzati ed installati su hardware Varian o d altre marche da essa indicate hanno le prestazioni descritte nel Manuale d uso fornito a corredo del software e
22. eliminare eventuali anomalie di funzionamento del software la Varian fornir 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 n 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 imp
23. for a few points in the gradient Suggestions For the 216 LC check the solvent levels in the A B and S pump reservoirs If the system has been sitting idle no flow run the flush air script to ensure that the pumps are properly primed Refer to the Proxeon 216 LC manual for more details on running maintenance scripts 18 Troubleshooting and Tips Daily Log Record instrument parameters and information about the analysis Review these entries to determine when parameters vary Record items such as e Emitter voltage e Backpressures of the trapping column and analytical column e Dates the columns were installed e Dates other components such as filters were installed Connections and Tubing Do not let the emitter dry out with sample inside it Precipitation causes blockage Before you store the emitter rinse the emitter with a clean solvent in which the sample is soluble Nanoscale connections are more critical than are conventional HPLC connections that use 1 16 inch OD tubing Even a small gap between a tube and a fitting can create a mixing volume that is detrimental to peak shape and resolution The small tubing inner diameters in nanobore are more susceptible to plugging so cleanliness is extremely important Many potential problems can be avoided by being careful when preparing and using the system Fused silica tubing is fragile Be very careful not to break crush or grind the ends Diagnosing Problems W
24. installed on 216 LC 0 50 uL Select based on the type of plate installed in the 216 LC Plate Options 4x6 2 mL Vials 8x12 96 well plate 16x24 384 well plate NOTE Recalibration must be performed if plate type is changed 38 Composition and Flow Toolbar In addition to the displayed tools click and drag a section of the x or y axis to zoom to a region The following table describes the icons Small Arrow hide or view the chromatogram toolbar Full Scale normalize the chromatogram vertically and horizontally Double click the lower left corner to do the same Vertical Scale normalize the chromatogram vertically Change the background color or display the background faded or solid Tile the chromatograms Overlay the chromatograms Method Builder The 216 LC has two Programs in Method Builder e Pump Program e Autosampler Wash Program ES Method1 E Method Notes Module 2 E LC nanoLC System Address 44 216 LC nanoLC System Control Address 44 Module Control Parameters Pump Program i Autosampler Wash Program Module Control Parameters Ef 500 MS Mass Spec Address 56 Pump Program ET 500 MS Mass Spec Control BE Autosampler Wash Program MS Acquisition Method Y Channel 1 Ms Data Standard MS Reports Print Options Results Format Chromatogram Format Compound Reports Last Modified Monday November 03 2008 16 52 34 2 Calibration Block Repo
25. offers advantages of increased sensitivity enhanced selectivity reduced interference and robust precise performance For a significant number of small molecule applications APCI may be the better solution than ESI Atmospheric Pressure Chemical lonization APCI requires the following e The liquid flow is rapidly vaporized e Solvent molecules are ionized in the corona discharge e Chemical lonization ionizes sample molecules The APCI process begins with pneumatically assisted nebulization of the LC eluent The spray of eluent droplets are completely vaporized in a hot turbulent flow of auxiliary gas The stream of vaporized mobile phase and sample components flows into the API chamber and crosses the path of a corona discharge Through a multi step process the corona discharge creates CI reagent ions from the large excess of mobile phase solvent molecules A final ion molecule reaction between these Cl reagent ions and neutral molecules of analyte generates the analyte ions the mass spectrometer monitors Positive lon APCI Positive lon APCI can occur as follows e Proton Transfer H30 M gt M H HzO Also CH3OH CH3CNH NH e Adduct Attachment NH M gt M NH Also CH3OH CH CNH H O e Charge Exchange Negative lon APCI Negative lon APCI can occur as follows e Proton Abstraction OH M gt M H H20 Also CH30 CH2CN e Adduct Attachment CH COC M M CH COO Also
26. out the narrow tip of the emitter positioned about 3 mm from the spray shield The solvent forms a Taylor cone due to the strong electric field At the tip of the cone charged solvent clusters are pulled into the gas phase This forms the visible plume that is observed with the camera Offline Analysis Offline analysis is well suited for introducing purified samples or simple sample mixtures in limited volume In offline analysis the electric field alone drives the sample flow The sample typically 1 5 uL is loaded into a single use emitter using a small diameter syringe needle or narrow pipette tip The emitter is placed into the holder and the high voltage is turned on This provides a continuous flow of the sample over an extended period For information on setting up the nESI source for offline analysis refer to the Appendix on page 47 Online Analysis In online analysis a pump delivers the sample to the emitter The pump may be a syringe pump or a nanoflow HPLC system A syringe pump is best suited for introducing purified samples or simple sample mixtures which are available in sufficient volume The use of a nanoflow HPLC system allows the separation and analysis of complex mixtures For information on setting up the nESI source for online analysis using a syringe for infusion see Installing an Online Emitter for Infusion Analysis on page 8 For information on setting up the nESI source for online analysis using a nan
27. protezione sicura m Assicurarsi che i coperchi delle lampade dei rivelatori a lunghezza fissa e variabile siano sempre al loro posto quando si lavora m 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 3 of 4 Disponibilit delle Parti di Ricambio E politica della Varian il fornire le parti di ricambio per lo strumento ed 1 suoi accessori per un periodo di cinque 5 anni a partire dalla data di produzione dell ultima unit della serie Le parti di ricambio saranno disponibili anche dopo questo periodo di cinque 5 anni ma solo in base alla disponibilit 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 perci sar possibile acquistarli dopo la Servizi Tecnico La Varian alla scadenza del periodo di garanzia in grado di fornire ai suoi clienti un ampia scelta di opzioni Le riparazioni possono essere effettuate sulla base di contratti di manutenzione particolar me
28. rigoureux par rapport des normes extr mement strictes reconnues au niveau international Nous sommes donc m me de vous garantir et de maintenir un niveau de qualit Lesdites proc dures ont re u l homologation ISO 9001 num ro FM21797 Les syst mes de qualit qui ont re u l homologation ISO 9001 pr sentent des avantages directs pour nos clients Nous sommes en mesure de vous livrer les instruments et de traiter les commandes en urgence dans des d lais record Nous r pondons pleinement et de mani re rapide vos commandes Nous avons mis en place un syst me de feedback continu de la part de nos clients et sommes conscients de vos attentes pr sentes et futures Nous avons am lior votre productivit en r duisant de moiti les Temps de panne et en acc l rant les temps de r ponse Nous avons apport des am liorations constantes au sein de notre structure afin d atteindre des niveaux de qualit optima l avenir Nos produits et services refl tent les exigences BPL pour vous permettre de r pondre aux imp ratifs de respect de la r glementation Toutefois nous ne nous contentons pas de l homologation ISO 9001 Pour nous la qualit est d finie par nos clients Nous ne sommes satisfaits que lorsque nos clients le sont Nous nous effor ons de comprendre vos besoins l aide d valuations externes de groupes d utilisateurs de comit s de conseil clients et de notre programme Hall
29. source septa colonnes fusibles papier graphique et encre n buliseurs cellules pistons joints raccords vannes br leurs tubes d chantillonnage inserts de sonde t tes d impression tubes garniture de verre dewars lignes de transfert disquettes cassettes magn tiques multiplicateurs d lectron filaments joints herm tiques isolant et toutes les pi ces en contact avec des chantillons et des phases mobiles Ladite garantie est nulle en cas d accident de mauvaise utilisation d alt ration de n gligence de bris d utilisation maintenance voire de modifications inappropri es d utilisation dans un environnement inadapt d utilisation avec une alimentation marginale ou d autres installations ou services inappropri s Un certain nombre de pr cautions doivent tre prises pour viter tout accident Ladite garantie se substitue et exclue express ment toute garantie expresse ou tacite y compris mais ne se limitant pas aux garanties relatives la qualit marchande du programme et la garantie de son aptitude une utilisation ou une application particuli re ainsi que toutes les autres obligations ou engagements de la part de Varian moins que lesdites garanties obligations ou engagements aient fait express ment l objet d un accord crit deVarian Limitations de garantie et de la responsabilit Les recours exclusifs du client sont express ment nonc s aux pr sentes En aucun cas Varian ne
30. the tests for removable radioactive contamination described in the Ni ECD manual m Comply with leak test schedules and procedures Burn Hazard Heated or cryogenically cooled zones of gas chromatographs can remain hot or cold for a considerable time after instrument power is turned off To prevent painful burns ensure that all heated or cooled areas have returned to room temperature or wear adequate hand protection before you touch potentially hot or cold surfaces LC Safety Practices High Pressure Hazard e Ifa 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 m Wear face protection when you inject samples or perform routine maintenance m Never open a solvent line or valve under pressure Stop the pump first and let the pressure drop to Zero m Use shatter proof reservoirs capable of operating at 50 60 psi m Keep the reservoir enclosure closed when the reservoir is under pressure m Read and adhere to all NOTES CAUTIONS and WARNINGS in the manual 03 914603 00 11 Flash Chromatography 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 Al
31. tighten the thumbscrew T Figure 6 10 8 Adjust the emitter position using the micrometer knobs on the nanospray chamber If you are replacing an existing emitter adjust the emitter position until the tip is visible in the camera image LX caution The Emitter tip may be damaged if it contacts the spray shield Positioning the Camera After the source is connected the LED light in the source turns on The light turns off when the chamber door is opened Use the light and the camera adjustment knobs to position the camera see Figure 1 The long edge of the camera image corresponds to approximately 2 mm 1 Move the camera forward until the edge of the spray shield can be seen to calibrate the emitter position 2 Move the emitter and chamber back in tandem to achieve a 2 3 mm gap between emitter and the spray shield In normal operation only the emitter and the spray plume are visible in the camera image Figure 6 After the initial setup leave the camera stationary After installing a new emitter move the emitter until it is visible in the camera image If the camera screen is black check for the following e The chamber door may be open and therefore the light is off e An emitter is not installed e The emitter is not in the field of view of the camera Adjust the system control and camera software displays to position them side by side so the spray and the spectrum are both in view 11
32. 00 2 We Flow Total Flow N A System Setup Hide Keypad Elution Status Not Ready A 87 2 bar B 92 0 bar 24 XB EI EM EA Activity Gradient Program Completed Pressure amp Flow v Instrument 1 Nov 11 13 13 22 Single Sample Completed Resume will continue the Open SampleLi Figure 22 31 Run Status Run Status Runtime 0 00 min Endtime 35 00 min Method 9 Ready No Fault Total Flow N A A 0 1 bar B 2 0 2 bar Run Status Item RunTime EndTime Status light Fault No Fault light Total Flow A B 96A B Buttons Item Method Reset ZA XB Description The elapsed time since the start of the run The time when the 216 LC Method will end Shows the state of the 216 LC The light will be red during pre gradient run activities During a gradient run or when idle the light will be green Shows whether the 216 LC has faults that have not been cleared The light appears green when the 216 LC has no uncleared faults otherwise it appears red The total flow of the solvent A and B pumps on the 216 LC Pressure of the A pump bars Pressure of the B pump bars Percent of the total flow made up from solvent pump A Percent of the total flow made up from solvent pump B Description Invoke the Method Builder and display the 216 LC Pump Program page of the active Method The 216 LC programmable parameters may then be modified Reset the module th
33. 00 3 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 Nz gas flows and temperatures to achieve maximum signal to noise Use the syringe pump with flow rates less than 100 uL min However at very low flow rates there can be arcing to the shield The vaporizer temperature is the most significant parameter lts optimum value is a function of e The sample experimentally determined e The mobile phase composition more water requires a higher temperature while a higher percentage of organic solvent requires a lower temperature e The flow rate higher flow rates require higher temperatures If the temperature is very low droplets will be observed at the outlet of the vaporizer tube If the temperature is too high the sample could thermally degrade Also important are the flow of the nebulizing and auxiliary gases as well as the temperature and flow of the drying gas Gas flows that are too low may cause an unstable baseline while gas flows that are too high may reduce the size of the observed peaks The vaporizer can be moved back in the spray chamber to decrease the likelihood of fouling the vacuum capillary when the matrix contains a large amo
34. 00 Series LC MS Quadrupoles Quad Control Window The following displays the features of the Quad Control Window that are unique to nanospray Click the Spray Chamber lower left or the Instrument Parameter upper right to open the Instrument Parameters dialog ua or Tose Renan vee ren gt Tune init Scan From Workstation modified Capillar y Oyringe 10ul etoppe LC Valve Load Ol vert Cannot find Instrument dri ver Set the nESI operating parameters in the API Source of the Instrument Parameters dialog Instrument Parameters E API Source Analyzer Safety Syringe Pump API Analyzer voltages off lonization mode API on off sequence Automatic nESI C Manual N2 Filing Time 10 Sec Equilibration time 10 Sec 3 Gases Diying gas 12 psi E fo E iso c e Heaters F API Housing 0 65 35 actual 0 C 0 on f Diyinggas 50 400 200 actual 0 C 0 on F Fo Figure 13 21 Method Builder In Method Builder click Acquisition Method to display the Method Specifications and Segment parameters Select nESI for lonization ES Method1 Method Notes FY Quad Mass Spec Address 42 PY Quad Mass Spec Control PY Acquisition Method Method Specs Model 320 GC amp LC v lonization nESI Click Advanced Options which is at the bottom of the method specifications Advanced Options Click the Emitter tab of the Advanced Options dialog Use the
35. 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 dr AS VARIAN www varianinc com 03 914603 81 11 Informations et mesures de s curit Instructions de fonctionnement Ce manuel d instruction est con u pour aider l utilisateur cr er des conditions op ratoires lui permettant de faire fonctionner le mat riel efficacement et en toute s curit Il contient entre autres certaines observations sp ciales pr sent es sous forme de NOTES MISES EN GARDE et AVERTISSEMENTS Il est important de faire fonctionner ce mat riel conform ment aux instructions du pr sent manuel et toute autre information manant de Varian S adresser au bureau r gional Varian pour toute question relative la s curit ou l utilisation correcte du mat riel NOTE Information destin e tirer le des performances A MISE EN GARDE A AVERTISSEMENT Attire l attention sur une situation Attire l attention sur une situation meilleur parti du mat riel sur le plan pouvant occasionner des dommages potentiellement dangereuse pouvant corporels l gers et ou des d g ts occasionner des dommages corporels mineurs l appareil et indique importants et indique comment comment rem dier cette situation rem dier
36. A Pr Varian Inc 2700 Mitchell Drive VA 2 l A N Walnut Creek CA 94598 1675 usa 1200 LC MS APCI Option Atmospheric Pressure Chemical lonization APCI Operator s Manual OVarian Inc 2003 2006 Printed in U S A 03 914981 00 Rev 3 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 2006 All rights reserved apy AS VARIAN 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 unl
37. CF HCOO e Electron Capture The APCI Source consists of two distinct parts the atmospheric pressure chamber and the API capillary assembly Vaporization ionization and desolvation occur in the atmospheric chamber The API capillary assembly uses a counter flow of drying gas to decluster heavily solvated ions Using optimized gas flows and electrical potential the API interface admits ions from the CI reaction while preventing neutrals from entering the sampling capillary 03 914981 00 3 Sample Inlet Meral Needle Quartz Tube u Heater Corona Needle mE 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 The intense pseudo molecular ion is however an ideal precursor ion for MS MS The requirements for volatility and thermal stability limit application of APCI to molecules below 1500 daltons Applications APCI is ideally suited to non polar and medium polarity molecules Analytes such as polynuclear aromatic hydrocarbons PAHS polychlorinated biphenyls PCBs fatty acids phthalates and triglycerides are perfect candidates for APCI The presence of one or more heteroatoms O N etc in an analyte increases the potential for the Cl reaction As such many drugs pesticides herbicides fungicid
38. E System Control Varian GC MS 1 Not Ready Fle Ede inject Automation Recalodate Instrument Windows Help dll Mtorgur00S3eamh rla kk a 300 MS 56 Not Ready Ri SiCamSWare 1 TC Manu Control Diagnostics Startup Shutdown Acqusiion Control and Status fr Method Active Segment Mode Amsbutes Optimization Pits Method Segment Method MC Upload MS Method EndTme 10 00 mirutes fV Detector On Scan Type 1005 ScanMode Enhanced Summory of Stohss F I Syinge Puro On Vacuum System OK Damong Gas OK Temperstures OK Source OK lon Gauge Pressure 00 uTom FAT Vaid General Parameters lonization Consol Nanospray lorizalion Parameters TuboDDS Parameters TuboDO5 Trigger F Entes Voltage Pondive 20002 vots F Doing Gas Pressure 1303 pa FF Spray Shand Voltage F Dying Gas Tempmatue 50 c Poste 3310 8 vota Warring Tempesahae changes of gestes thon FT a 45 deg C may result in longer stabiizaion times Relays rarerara e Hale kemea PT Select Views E Port Valve Ion Gauge Sof Dear 0 Postion 1 pann Sp ud ad ea O Poster 2 AJ elo aj 11 m Scan Number 3347 Time 23 993 min Base Peak 268 9 Base Amount 23 RIC 8535 lon Range 95 7 2756 mz lon 250000 us Segment 1 Channel 2 po I T 7 Acijored Range nis Instrument 1 Jul 18 13 47 56 Ins 1 Module 44 Module READY Figure 7 Positioning an Online Emitter Look through the front and top windows of the spray chambe
39. Emitter tab to set the ramping parameters of the emitter voltage during a run Positive Emitter Voltage Program MN Positive Emitter Voltages Programs in use Volts Times minutes Initial Initial Hold Time 2000 0 oo Rate V min Final Hold Time o Total run time 0 0 Min a Negative Emitter Voltage Program IV Negative Emitter Voltages Programs in use Volts Times minutes Initial Initial Hold Time Rate Y min Final Hold Time ri Total run time 0 0 Min a Figure 14 22 Use the Overrides tab to set override values for the Positive and Negative Emitter Voltage the Negative and Positive Spray Shield Voltage and the Spray Chamber Temperature for specific segments If no overrides are checked the values used are those set in the Instrument Parameters dialog Use Reset to defaults override E Detector 1000 Y Copy to all E Emitter Voltage Positive 2000 Y Copy to all E Emitter Voltage Negative 2000 Y Copy to all E Spray Shield Voltage Positive 30 v Copy to all E Spray Shield Yoltage Negative 30 Y Copy to all E Spray Chamber Temperature E Figure 15 23 24 500 MS lon Trap System Control In the Control and Status view the Source readback is determined from the spray chamber The software only opens methods compatible with the installed source Control and Status MethodnESI Upload MS Method Click the Nanospray lonization Parameters tab from the Active Seg
40. Flow Toolb t 2 sects rtp don amis him eue anni 39 Method Bulld6l irr a em eo tue mut per ten ce a vec e ran Pera 39 216 LG Pump Program Window ecc p RERO te RR ene Let ee gr eee CAE E acd 40 Flow Composition Time Program usines 40 Equilibration Programs tests e cte me eves coner a est d eee tin P ede 41 216 LC AutoSampler Wash Program Window sien 43 Spare Pals 45 A oat DIAM IARE S DD E Niere ERIS E E I D IRIS 47 Offline Emitters ta EE 47 Specifications E E 47 Operating the Offline Emite ocacion 47 Offline Emitter Entstehung tese lerne 48 Introduction Overview The Varian nanoelectrospray ionization nESI source extends the use of ESI to low flow rates While nESI can introduce the same types of samples to the mass spectrometer as standard ESI some of the hardware is different and some parameters have different ranges Parameter ESI nESI Typical flow rate 200 uL min 300 nL min Typical column ID 2 mm 0 075 mm Spray needle inner diameter 100 150 um 1 30 um Distance from needle to spray 10 20 mm 2 3 mm shield Nebulizing gas 1 2 liters min Not used Spray voltage 5000 V 2000V The absence of nebulizing gas makes the position of the spray needle called the emitter in nESI much more critical The built in camera and precision stage adjustments allow fine positioning of the emitter There are two ways to do nESI e Offline e Online For both techniques the solvent flows
41. N Le alerta de potenciales situaciones peligrosas que pueden causar serios situaciones Descripci n El instrumento utiliza voltages peligrosos Desconecte el interruptor general antes de retirar los paneles atornillados Peligro de productos qu micos Evite el contacto especialmente cuando rellene los dep sitos utilice protecci n de ojos y piel Superficies posiblemente calientes 6 fr as criog nico Utilice protecci n para la piel Las part culas vol tiles productos qu micos o radiaci n UV pueden causar da os en los ojos Usar las debidas protecciones para la cara y los ojos Peligro potencial de fuego Siga las instrucciones del Manual de Operaci n para su seguro funcionamiento Peligro potencial de explosi n debido al tipo de gas l quido empleado Peligro por Fuente de radiaci n Siga las instrucciones del Manual de Operaci n para su seguro funcionamiento Mantenga alejados los dedos y las manos Ar AS VARIAN 10f4 Precauciones Generales de Seguridad Siga estas indicaciones de seguridad para una correcta operaci n del equipo Realice verificaciones peri dicas de fugas en todas las l neas de suministro y tuber as No permita que las l neas de gas se doblen pinchen Mant ngalas alejadas de zonas de paso y del calor fr o excesivo Guarde los disolventes org nicos en cabinas ventiladas a prueba de fuego y etiquetadas para que puedan ser f cilmente identificadas como mater
42. ace 2 Tighten the thumbscrew to hold the conductive union in place 3 Start the nanospray pump with an isocratic flow that is at least 50 organic Refer to the Proxeon 216 LC manual 4 After the LC pressure stabilizes check for flow out of the emitter and examine each connection for leaks If bubbles are observed the spray in the camera image stops and a small droplet forms on the end of the emitter air may be trapped in the connectors and tubes Wait several minutes for the air to leave NOTE Increasing the organic percentage of the mobile phase helps to remove air bubbles trapped in fittings by decreasing the surface tension 5 Determine the flow rates for the equilibration and sample loading step for the trapping column 6 Determine the flow rates for the analytical column Both should be 200 bar or less to compensate for column aging and room temperature fluctuations and the highest allowable flow rate while keeping the pressure at 200 bar or less Determine the optimum emitter voltage at 50 acetonitrile Determine the optimum emitter voltage again at 10 acetonitrile Build the workstation method with the parameters determined in the previous steps 10 To inject a sample select the Inject Single Sample icon or begin a sample list 11 Check the sample list to ensure that the correct flows and volumes for the sample pickup and loading were entered Table 1 Recommended Starting Parameters for the 216 LC System
43. an consiste fournir des pi ces de rechange pour tous les appareils et accessoires majeurs durant une p riode de cinq 5 ans apr s livraison de leur production finale Les pi ces de rechange ne sont fournies au terme de cette p riode de cinq 5 ans que suivant les disponibilit s Il faut entendre par pi ces de rechange les pi ces individuelles lectriques ou m caniques susceptibles de d faillance au cours de leur utilisation normale Par exemple les relais les lampes les sondes thermiques les l ments de d tecteur les moteurs etc Les parties en t les les l ments ou assemblages structurels et les pi ces de fonderie les cartes circuits imprim s et les modules fonctionnels sont normalement susceptibles d tre remis l tat neuf pendant toute la dur e de leur vie utile et ne sont d s lors fournies au terme de la production finale des appareils que suivant les disponibilit s Service d assistance la client le Varian fournit divers services destin s aider sa client le apr s expiration de la garantie service de r paration sur base de contrats de maintenance prix attractifs ou sur base d accords dur e limit e portant sur du mat riel sp cifique support technique et service de formation assur s par des chimistes qualifi s sur base contractuelle ou en fonction des besoins sp cifiques Points de vente des instruments analytiques Varian Contactez votre point de vente r gional Va
44. braci n no afecte al trabajo del detector m Compruebe peri dicamente el correcto funcionamiento del sistema m Asegurese de una correcta ventilaci n del laboratorio Detectores con fuentes radioctivas m Leaconcuidado y cumpla todas las NOTAS PRECAUCION y ATENCION del Manual del Detector Ni ECD m Realice los test de contaminaci n radioactiva descritos en el Manual del Detector Ni ECD m Cumpla con los plazos y procedimientos de test de fugas Peligro de Quemaduras Las zonas de calor 6 fr o criog nicas del Cromat grafo de Gases pueden permanecer calientes fr as durante bastante tiempo despu s de apagar el instrumento Para evitar quemaduras asegureses de que todas las reas que se calienten 6 enfr en han vuelto a la temperatura ambiente protejase adecuadamente las manos antes de tocar las superficies potencialmente calientes 6 fr as LC Pr cticas de Seguridad Peligro de Alta Presi n Si se rompe una l nea de presi n se abre una v lvula de seguridad accidentalmente bajo presi n la bomba puede generar l quidos a alta presi n potencialmente peligrosos produciendo un chorro a alta velocidad de l quidos vol tiles y t xicos m Lleve protecci n facial cuando inyecte muestras 6 realice mantenimiento de rutina 03 914603 84 11 m Nunca abra una l nea 6 una v lvula bajo presi n Apague la bomba antes y deje que la presi n baje a cero m Utilice dep sitos irrompibles qu
45. cetonitrile have lower surface tensions than mobile phases that have a high percentage of water Mobile phases with lower surface tensions allow smaller droplets to form which results in a consistent spray plume Figure 9 Spray plume with a high percentage of organic mobile phase 14 The difference in optimum voltage between high and low water concentration is generally only a few hundred volts for a new emitter but may be more for a used emitter For an extremely rounded emitter one with many hours of use it may not be possible to get a stable spray with a highly aqueous mobile phase After the tip rounds replace the emitter Remove deposits from the exterior of the emitter tip by gently wiping with a lint free laboratory wipe Take extreme care not to bend or break the emitter Using a Column and Nanoflow LC Overview This is an overview of using the Varian 216 LC system with a nanobore column Complex samples require chromatographic separation before the components are analyzed with the MS The 216 LC is optimized for separating the peptides produced by an enzymatic protein digest A trapping column must be used to concentrate the sample for the following reasons First the permeability of the trapping column is much higher than that of the analytical column which allows the contents of a 20 uL sample loop to be flushed onto the trapping column in a few minutes using a flow rate much higher than the analytical flow the fl
46. connect the 216 LC directly to the back of the MS a Forthe 320 MS enable a Start In Signal as shown in Figure 19 in the Configuration Sync Signals Quad MS Toolbar menu Start In Signal V Enabled C VarianGC Cable 03 937179 01 GC QuadMS ve Generic Cable 03 937413 01 Generic QuadMS or Wing Generic 10 Board Assembly CUB06 00047 If the instrument is ready to acquire data closing the f Looking for an up edge contact between Pins 2 and 3 at Row 1 Column A C Looking for a down edge of the 10 connector will start an acquisition Figure 19 2 Configure the Connections screen of the 216 LC as shown dE proxeon 0 EB ESTER at GEN PROXEON Home Batch Setup Method Editor Maintenance Configuration Users Mass Spectrometer Connections f Instrument Generic Network Time Communications Use Contact Closure Backup Contact Closure Settings EASY nLC Generic Protocol OUT State at start IN 4 OUT2 Start at IN2 tart In Job 00 47 46 3 7 OUT3 4 Sample 00 47 47 Signal width E TTL Gradient 25 00 J GND 11 Now 2008 1410 Press to logout p AG S admin Figure 20 29 Configuring MS Workstation with the 216 LC 1 Select Set up Ethernet Communication from the Instrument Menu on the MS Workstation toolbar 2 Select Module Type and enter the correct IP Address The IP Address should match the IP address that is configured on
47. ctor from the front panel of the instrument The socket is marked API Housing Disconnect the small 4 pin round connector from the socket marked APCI Heater With the spray chamber still closed and latched loosen the two screws on top of nebulizer The nebulizer has the heat sink fins Remove nebulizer assembly 03 937326 01 by lifting straight up Set it aside carefully so nebulizer tube does not get damaged or bent Carefully remove the black O ring 03 930109 06 from the end of the quartz tube 03 914981 00 3 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 After checking that the vaporizer has cooled loosen and remove the threaded compression fitting 03 937340 01 from the end of the vaporizer tube inside the spray chamber 14 Carefully pull the quartz tube out the bottom of the vaporizer the end in the spray chamber Be sure to keep the tube in line with the heater as you pull it out Do not tilt it to the side Use a slight twisting motion if the tube binds within the heater The ferrule will remain attached to the tube Discard both the quartz tube and the ferrule Installing the Quartz Tube 1 Close and latch the spray chamber 2 Place the white cera
48. curit Les pratiques suivantes garantissent une utilisation sans risques du mat riel Effectuer r guli rement des essais d tanch it de tous les conduits d alimentation et de tous les tuyaux du syst me pneumatique Ne pas travailler avec des conduits de gaz d form s ou perc s Installer les conduits de gaz l cart des all es et venues et l abri du chaud ou du froid Conserver les solvants organiques dans des r cipients l preuve du feu bien ventil s 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 liminer conform ment un programme agr d limination des d chets et non via les gouts municipaux NOTE Ce mat riel a t test conform ment aux dispositions de la directive CME afin de pouvoir porter le sigle CE de l Union europ enne Il en r sulte qu il peut tre sensible des niveaux de radiation d interf rence ou des fr quences se situant hors des limites test es Ce mat riel est con u pour effectuer des analyses chromatographiques d chantillons ATTENTION pr par s selon des m thodes appropri es Il convient de le faire fonctionner avec les gaz maximales sp cifi es dans le pr sent manuel Le client est tenu d informer le service Varian d assistance la client le que son mat riel et ou les solvants ad quats et dans les limites des pressions de
49. d tanch it Risque de br lures Les zones des chromatographes gaz chauff es ou trait es cryog niquement peuvent rester tr s chaudes ou tr s froides durant une p riode plus ou moins longue apr s la mise hors tension du mat riel Pour viter les br lures s assurer que ces zones sont revenues temp rature ambiante ou utiliser un dispositif ad quat de protection des mains avant de les toucher Mesures de s curit en CPL Risques li s aux hautes pressions En cas de rupture d un tuyau ou en cas d ouverture accidentelle d une vanne alors que le syst me est sous pression la pompe peut occasionner des dommages en expulsant grande vitesse des jets de liquides volatiles et ou toxiques m Mettre un masque de protection lors de l injection des chantillons ou en effectuant les op rations de maintenance de routine 03 914603 82 11 m Ne jamais d connecter un conduit de solvant ou une vanne sous pression Arr ter pr alablement la pompe et laisser la pression descendre z ro m Utiliser des r servoirs incassables 50 60 psi m Laisser l enceinte du r servoir ferm e lorsque le r servoir est sous pression m Se conformer aux NOTES MISES EN GARDE ET AVERTISSEMENTS du manuel d utilisation Chromatographie Flash L utilisateur aura la connaissance des propri t s physico chimiques des constituants de la phase mobile Eviter le contact direct des solvants avec les tuyaux en polyur thane cer
50. d meer aa ete des 15 COMAS nern teet e RE er aed ne ee SE cuc ria tuus 16 Optimizing Operating Parameters sise 17 Optimizing the Drying Gas Flow Rate siennes 18 Troubleshootng and Tips aa 19 E e e PPPA 2 STE M 19 Connections and TOBING E RA a ara 19 Diagnosing Problems eee A A rame an ln 19 BIOCKAQES m 19 R EL D POTITO 20 succ 20 Troubleshooting Guides doeet e ee toe a e e fe an 20 300 Series LC MS Quadrupoles sess 21 Quad Control WindOoW ici re qe E aeta ee tiesa 21 Method B llder z 42 22 rendered e bebe idet tte ab p eid epus 22 500 MS Ton TAPER NUR 25 SYStEM Cont ci ms 25 Method Builders ccc irreali fede ceo oe epe Lee 26 PAP EON TD 29 Configuring the 216 LC with MS Workstation sise 29 Configuring the 216 LC for MS Workstation Control 29 Configuring MS Workstation with the 216 LC eee ns snnnnnennnnnnennnnnnnnnnnnnnennnnnnnennnnnnennnnnnnn nn nnn ern 30 216 LC Status and Control Window 2 en er ne ah ae ad 31 RUNAS dd ed da nn ct Ne 32 P tnp Status ca en mn ci adele ila de eta iaia 33 Valve STATUS tao 33 Elution Status and Activity caido 34 Button Barr EE 34 AutoSampler Plate Display ui iia n t nto in cdi tr 35 Pressure Flow and Composition Plots iii 35 GLP Dialog BOX sti erre Riel alal ea hail mittet hei 37 216 LC SampleList Window Extensions eee 38 Hardware Dialog BoX uan o ee ed 38 Composition and
51. d the achieved flow rate is around 15 100 nL min Offline Emitter specifications OD 1 2 mm Length 5 cm Tip must have conductive coating Thumbscrew PN 1280830300 Emitter Hold Spring N PN 393274001 Offline Emitter 1 2 mm OD with tip coating Not included in accessory kit Holes for Mounting Screws Offline Emitter Holder 393274001 Operating the Offline Emitter 1 Remove the online emitter union clamp from the clamp platform by loosening the two mounting screws 2 Install the offline emitter holder on the clamp platform 47 3 Use a fused silica needle or a gel loading tip to load the sample into the emitter Place the emitter into the holder using the spring to hold it in place Put the tip of the emitter 2 3 mm away from the spray shield 6 Aim the tip of the emitter toward the upper half of the hole in the spray shield The star marks the spot Spray shield View through front window 7 Start at 1400V and gradually increase the emitter voltage until the spray is stable Offline Emitter Hints Adjust the voltage to the minimum voltage required to produce a stable flow Increasing the voltage beyond this value will increase the flow rate and sample consumption without an increase in signal intensity An extremely high voltage will sputter the conductive coating from the tip caution Use care when handling the offline emitters as both the tip and the conductive coating
52. dom 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 dr 2 VARIAN www varianinc com 03 914603 83 11 Instrucciones de Operaci n Instrucciones de Seguridad Este Manual de Instrucciones est dise ado para ayudarle a establecer las condiciones de operaci n que le permitan operar su instrumento de forma segura y eficaz As mismo se describen consideraciones especiales 6 precauciones que aparecen en forma de NOTA PRECAUCION y ATENCION como se indica m s abajo Es importante que utilice el instrumento de acuerdo con este Manual de Operaci n y cualquier otra informaci n que le proporcione Varian Remita a la Oficina Local de Varian cualquier cuesti n que tenga respecto al correcto uso de su equipo NOTA Informaci n para ayudarle a obtener unas prestaciones ptimas de su instrumento S mbolo ATENCI N PELIGRO DE DESCARGA ELECTRICA ATENCI N PELIGRO QU MICO ATENCI N PELIGRO DE QUEMADURAS ATENCI N PELIGRO PARA LOS OJOS ATENCI N PELIGRO DE FUEGO ATENCI N LA PELIGRO DE EXPLOSI N PA ATENCI N PELIGRO DE RADIACION A ATENCI N PARTES EN MOVIMIENTO 03 914603 84 11 Le alerta de situaci nes que pueden causar da os moderados a la salud 6 al equipo y c m evitar esas da os y c mo evitar esas situaciones PRECAUCION ATENCI
53. e MS with ESI source before proceeding with nESI installation To attach the nESI ion source 1 Close System Control 500 MS only not necessary for 320 MS 2 Install the nESI spray shield Spray Shield 3 Insert the hinge rod of the nESI ion source into the slot at the bottom of the vacuum interface plug on the front MS and pull back so that the rod is captured in the slot Close and latch the ion source Open the lower front cover of the instrument Connect the electrical cables a Large 14 pin round connector to the API housing socket b High voltage cable to the emitter voltage connection Installing and Operating the Camera Installing the Camera Software For more details about installing the camera and software see the Quick Start Reference Guide in the USB Color Camera User s Manual which is on the MS Workstation CD 1 Open the Camera folder on the MS Workstation CD 2 Run setup exe 3 Follow the prompts 4 Accept the default location c Program Files StCamSWare If an error message about the lack of Windows Logo testing opens click Continue Anyway Connecting the Camera After installing the camera software do the following 1 Connect the camera to the USB port 2 The Found New Hardware Wizard opens Click No not at this time to instruct Windows not to connect to Windows Update Select Install the Software Automatically If you get an error about lack of Windows Logo testing click C
54. e needs if it is bent damaged or cannot be cleaned satisfactorily Remove the corona needle by grasping it with your fingers and pulling it straight out of its mount Be careful of the sharp point Insert a new or cleaned corona needle into the mounting hole and press firmly until it is fully seated The alignment should not change during normal needle cleaning or replacement The needle is properly aligned when there is 1 cm between the end of the needle and the end of the vaporizer assembly While firmly holding the corona needle mount loosen the set screw in the mount with a 1 5 mm hex key and rotate the needle mount until the needle is 1 cm below the vaporizer assembly and then retighten the set screw Do not remove the set screw from the mount Do not remove the needle mount from the high voltage standoff Hold the needle mount firmly while making adjustments 12 03 914981 00 3 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 Installation Carefully feed the new needle assembly 03 937544 03 into the hole in the nebulizer assembly being careful not to bend the new needle Slide a ne
55. e sean capaces de operar a 50 60 psi m Mantenga cerrada la junta del dep sito cuando se haye bajo presi n m Lea y cumpla todas las NOTA PRECAUCION y ATENCION del manual Cromatograf a Flash El operador debe familiarizarse con las propiedades f sico qu micas de los componentes de la fase m vil 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 explosi n Todos los componentes del sistema deben estar conectados a un enchufe com n con toma de tierra com n Esta toma de tierra debe ser una toma de tierra verdadera en lugar de flotante Los disolventes no polares pueden originar carga est tica cuando son bombeados por el sistema Todos los recipientes que contienen fase m vil incluyendo los tubos y los recipientes de recogida deben estar conectados a tierra para disipar la electricidad est tica Utilizar medidores de carga est tica y los debidos dispositivos de descarga por Ej ionizadores de aire para salvaguardarse contra la creaci n de electricidad est tica Radiaci n Ultravioleta Los detectores del Cromat grafo de L quidos que utilizan una fuente de luz ultravioleta disponen de protecci n para prevenir exposiciones radioactivas al personal Para una correcta protecci n m Asegurese de que las cubiertas de protecci n de la l mpara de los detectores est correctamente
56. e 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 2 of 4 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 qualit Usare solo tubazioni cromatograficamente pulite Numero di Parte Varian 03 918326 00 e calibrate per pressioni superiori a quella massima di uscita dal manometro 03 914603 83 11 Procedure di Sicurezza in GC Scarico dei Gas Per i rivelatori GC non richiesto alcun sistema particolare di scarico dei gas se lo strumento installato in una stanza ben ventilata e se non viene utilizzato per l analisi di sostanze chimiche pericolose Se si deve installare un sistema di scarico dei gas m Usare condutture no
57. eable 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 03 914412 00 2 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
58. eaks are observed but the background spectrum looks normal the temperature may be set too low for the sample If smaller than expected peaks are observed or the peak shape shows extreme tailing the temperature may be set too low If the background spectrum has no ions try increasing the corona current If operating in negative mode be sure the nebulizing gas is air If condensation is observed in the spray chamber the housing temperature may be too low for the flow conditions or there has been insufficient warm up time If the baseline is noisy it may be as a result of poor nebulization Check the gas flows and temperatures If the baseline is noisy and or elevated the chamber may need cleaning or the mobile phase may be contaminated If liquid drops are seen at the end of the quartz tube it may be because the mobile phase contains a high percentage of water flowing at a high flow rate Increase the vaporizer temperature or reduce the flow rate until the drops are no longer visible If intense mass peaks are observed in the background spectrum even without liquid flow try cleaning then baking out the spray chamber at maximum temperature for 2 hours If the contamination still persists then the O rings which seal the chamber and or the chamber windows may be contaminated and should be replaced If the vaporizer temperature does not increase when turned on contact your local Varian Inc representative for instrument repair and
59. eistungen an Reparaturservice kann zu attrak tiven Preisen ber eine Wartungs vereinbarung oder nach Zeit und Materialaufwand zur Verf gung gestellt werden Technische Unter st tzung und Training bieten wir Ihnen durch qualifizierte Chemiker sowohl auf einer Kontraktbasis als tionsauslauf des Instruments geliefert werden auch nach Ihren Erfordernissen an Varian Analytical Instruments Verkaufsb ros F r Verkaufs oder Servicehilfe und zum Bestellen von Teilen und Zubeh ren setzen Sie sich bitte mit Ihrem Varian B ro in Verbindung Argentina Buenos Aires Tel 54 11 4 783 5306 Australia Mulgrave Victoria Tel 61 3 9566 1134 Austria V sendorf bei Wien Tel 43 1 699 9669 Benelux Bergen Op Zoom Tel 31 164 282 800 Brazil and Latin America S S o 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 4 of 4 France Les Ulis C dex 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
60. ent 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 V sendorf bei Wien Tel 43 1 699 9669 Benelux Bergen Op Zoom Tel 31 164 282 800 Brazil and Latin America S Sao 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 4 of 4 France Les Ulis C dex 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 ap AS VARIAN www varianinc com 03 914603 00 11 Arbeitsanleitungen Sicherheitsinformationen Diese Arbeitsanle
61. ento stato testato secondo le Direttive EMC allo scopo di poter utilizzare il Marchio CE della Comunit Europea Questo strumento pu essere suscettibile a radiazioni interferenze o frequenze che non sono entro i limiti collaudati preparati Deve essere utilizzato usando gas e solventi adatti a questo scopo ed entro i limiti Questo strumento progettato per l analisi cromatografica di campioni opportunamente AN ATTENZIONE massimi di pressione flusso e temperatura riportati in questo manuale Se lo strumento non viene utilizzato secondo le modalit specificate dal costruttore le condizioni di sicurezza previste potranno non essere sufficienti intervento di riparazione se lo strumento stato utilizzato per l analisi di campioni E responsabilit del Cliente informare il Servizio Tecnico Varian prima di qualsiasi A ATIENZIONE 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 polarit riportate nel manuale di istruzioni che quelle stabilite dalle norme di sicurezza del laboratorio Sostituire i fusibili bruciati solo con fusibili che abbiano le stesse caratteristiche queste ultim
62. er Abgasf hrung m Sorgen Sie f r gute Entl ftung im Laborbereich Radioaktive Detektoren m Lesen Sie sorgf ltig und befolgen Sie alle HINWEISE ACHTUNGEN und WARNUNGEN im Ni ECD Handbuch m F hren Sie die Tests f r zu beseitigende radioak tive Kontamination durch die im Ni ECD Hand buch beschrieben sind m Erfiillen Sie die Zeitpl ne und Verfahren zur Di chtigkeitspr fung Verbrennungsgefahr Beheizte oder tieftemperaturgek hlte Zonen des Gas chromatographen k nnen betr chtlich lange heif oder kalt bleiben nachdem das Instrument bereits abgeschal tet ist Zur Vermeidung schmerzhafter Verbrennungen m ssen Sie darauf achten da alle beheizten oder gek hlten Zonen auf Raumtemperatur zur ckgegangen sind oder Sie m ssen ausreichenden Handschutz be nutzen bevor Sie m glicherweise hei e oder kalte Oberfl chen ber hren LC Sicherheitspraktiken Gefahr durch hohen Druck Wenn eine Leitung bricht eine Entl ftungseinheit sich ffnet oder ein Ventil sich unbeabsichtigt unter Druck ffnet kann durch die Pumpe m glicherweise ein ge f hrlich hoher Fl ssigkeitsdruck entstehen der einen Strahl fl chtiger und oder toxischer Fl ssigkeiten von hoher St mungsgeschwindigkeit verursacht m Tragen Sie einen Gesichtsschutz wenn Sie Proben injizieren oder Routinewartungen durchf hren 03 914603 81 11 m ffnen Sie niemals eine unter Druck stehende L sungsmittelleitung oder ein Ventil Halten Sie zue
63. er Qualit tsbestimmungen zu entwirren Diese Standards legen ein Modell f r Qualit tssicherungssysteme hinsichtlich Produktdesign Entwicklung Herstellung Installation Service und Kundenbetreuung fest Sie sind nun die weltweiten MaBst be der Qualit tssicherung die die An strengungen eines Unternehmens bez glich der Qualit t und der Bedeutung seiner Qualit tssysteme mes sen Verschiedene Organisationen in der ganzen Welt wie die British Standards Institution BSD stel len ausgebildete objektive Pr fer zur Begutachtung von Qualit tsma nahmen Produktentwicklung Her stellungsprozessen und von Programmen zur Erforschung der Kundenzufriedenheit zur Verf gung Kein Unternehmen kann die ISO 9000 Registrierung beantragen ohne die Genehmigung von den beauftragten Qualit tsgutachtern der BSI oder einer hnlichen akkreditierten Stelle erhalten zu haben Die ISO 9000 Registrierung bildet einen objektiven Bericht von dritter Seite um den Grad der Qualit tsanstrengung 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 da jedes Stadium unseres Qualit tssystems einschlieBlich Produktentwicklung Herstellung Endkontrolle Versand sowie Teile und Zubeh r rigoros gegen die anspruchsvollste Serie international anerkannter Standards gepr ft worden ist Das bedeutet da wir einen Qualit tss
64. er than 100 uL min depending on the column 41 Analytical Column Re Equilibration Volume uL 0 to 137 0 uL Total volume to flow though the column during the equilibration phase Specify a 0 volume to omit this phase Flow uL min 0 01 to 100 0 uL min Flow rate to use during equilibration Note that Pmax may be reached at a flow much lower than 100 uL min depending on the column Maximum Pressure Pressure bar to 300 bar The System stops during any phase of the analysis cycle if the pressure reported by the A or B pump exceeds this limit 42 216 LC AutoSampler Wash Program Window Autosampler Wash Options Wash Volume uL MW Use Custom Wash Program Source Volume uL Cycles Add Item Description Wash Volume uL 30 100 uL Specify a volume for the wash step Use Custom Wash If enabled the program is used instead of the Wash Program Volume The program has a maximum of 10 steps Source For each step specify the wash vial Volume uL Volume for each wash cycle Cycles Number of times this wash step is preformed 43 44 Spare Parts Screw pan 3x0 5x12 mm UCF112 Spare ferrule 1 32 in UCP659 Luer syringe adapter UCFS120 Fused silica tubing 20 pm ID UCFS150 Fused silica tubing 50 pm ID 45 46 Appendix Offline Emitters Specifications Generally the inner diameter of offline emitter tips is smaller than the inner diameter of online emitter tips on the order of 1 4 um an
65. es and natural products can be analyzed with APCI Highly charged thermally unstable and large molecular weight analytes should be avoided These compounds are unacceptable as analytes and should also be avoided as matrix components since the lack of volatility and degradation products may increase maintenance of the APCI vaporization assembly and chamber Atmospheric Pressure Chemical lonization 5 Installation of APCI Chamber 1 Remove the Electrospray lonization ESI chamber if installed WARNING Source parts become hot during operation Use caution when BURN HAZARD installing or removing the API Source 2 Connect the gas lines to the nebulizer assembly Nebulizing gas top fitting Auxiliary gas bottom fitting Needle Gas Green Nebulizing Gas APCI Aux Gas Yellow N2 Connection to Drying Gas Red API Plug N2 Connection to Aux Gas Yellow APCI Only N2 Connection to Needle Gas Green Nebulizing Gas ESI 8 APCI 3 Connect the large 14 pin round connector to the socket marked API Housing 4 Connect the small 4 pin round connector to the socket marked APCI Plug 03 914981 00 3 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 3 Se
66. ess 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 embedd
67. fiillen der Reservoirs Benutzen Sie wirksamen Augen und Hautschutz Sehr hei e oder tiefstgek hlte Oberfl chen k nnen freigelegt sein Benutzen Sie einen wirksamen Hautschutz Herumfliegende Partikel Chemikalien oder UV Strahlung k nnen Augensch den verursachen Tragen Sie deshalb einen geeigneten Schutz f r Augen und Gesicht Es besteht eine m gliche Feuergefahr Beachten Sie die Vorschriften im Handbuch f r eine gefahrlose Benutzung Eine m gliche Explosionsgefahr besteht infolge der benutzten Gas oder Fl ssigkeitsart Es besteht eine ionisierende Strahlungsquelle Beachten Sie die Vorschriften im Handbuch f r eine gefahrlose Benutzung Bleiben Sie mit Ihren H nden und Fingern weg Ar A VARIAN 1of4 Allgemeine SicherheitsmaBnahmen Befolgen Sie diese Sicherheitspraktiken f r eine gefahrlose Ger tebenutzung Pr fen Sie regelm ig alle Versorgungs und Pneumatikleitungen auf Lecks Gasleitungen d rfen nicht geknickt oder angestochen werden Verlegen Sie die Leitungen au er halb von Laufwegen und abseits von extremer Hitze oder K lte Lagern Sie organische L sungsmittel in feuerfesten bel fteten und eindeutig bezeichneten Schr nken damit sie leicht als toxische und oder brennbare Materialien erkannt werden Sammeln Sie keine L sungsmittelabf lle Entsorgen Sie solche Materialien ber ein geregeltes Ent sorgungsprogramm und nicht ber die ffentlichen Abwasserleitungen HINWEIS Dies Inst
68. fill Indicates the well vial currently being sampled Blue fill Indicates the wells vials in the active SampleList that have been sampled Pressure Flow and Composition Plots The 216 LC System can display e composition display for the B pump e pressure trace for the A and B pumps e flow display for the A and B pumps The display format is controlled by the following menu 35 System Setup Hide Keypad t Pressure amp Flow Composition amp Pressure amp Flow Composition The Composition Plot shows B vs time during the gradient time program At the start of the gradient only the method program is displayed and the achieved B trace is overlaid as the run progresses The Pressure and Flow displays for both pumps share the same time base corresponding to the complete analysis cycle starting with the pre column equilibration Flow and pressure panels can be stacked or overlaid Vertical annotations indicate the transitions between the major phases of the cycle doi System Control NanoSpray System 1 Suspended E Pu St DER Fie Edt Inject Automation Recalculate Instrument Wir Inj Hel File F Option O a sis Bisso fu mh gt al e S BA BE n m Capture C Window W Help H 216 LC 44 Ready Run Status Pump Status Valve Status Runtime 0 00 min Reset Pump Flow Setpoint Actual Flow Pressure bar Available Volume uL Flow Endtime 25 00 min A 0 0 nL min 85 5 nL m
69. grado d impegno di una determinata azienda nei confronti della qualit Nel 1992 la Varian Inc Analytical Instruments ha ottenuto l omologazione allo standard pi completo della serie ISO 9000 l ISO 9001 L omologazione ISO 9001 significa che ogni singola fase del nostro sistema di qualit compresi lo sviluppo del prodotto la fabbricazione le prove finali la spedizione i componenti e le forniture stata rigorosamente esaminata a fronte della serie pi esigente di standard riconosciuti a livello mondiale il che significa che rispondiamo pienamente ad uno standard qualitativo sul quale il cliente pu contare oggi come nel futuro Il nostro Sistema di Qualit ha ottenuto la certificazione ISO 9001 col numero FM21797 I sistemi di qualit 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 pi rapidamente rispetto al passato con la possibilit di evadere le richieste d emergenza con una rapidit 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 produttivit del cliente riducendo della met il tasso di guasti dei sistemi e velocizzando i tempi d intervento della manutenzione Abbiamo intr
70. hen you have a problem review your recent actions For example if you just installed a new column check those fittings first When you suspect a problem measure the pressure at several flow rates If the pressure is not proportional to the flow rate then there is a problem The 216 LC has maintenance scripts such as the leak test which are helpful Blockages To find a blockage working from the emitter toward the pump or syringe loosen fittings one at a time until the pressure drops 19 Leaks To find a leak work from the pump or syringe toward the emitter and check that each fitting is seated properly before retightening the fitting A sleeve must extend about 1 5 mm through the ferrule and the emitter must be flush with the end of the sleeve If the sleeve does not extend that far push it out farther and reassemble the fitting while keeping the emitter flush with the end of the sleeve The flow rate of a few hundred nanoliters per minute means that it takes a leak several minutes to create a visible drop Some types of fittings leak after several minutes of pumping while others collect a very large volume before you can see liquid Bubbles Air may be in the fittings before they are connected to the flow path and it may take several minutes to flush it out Troubleshooting Guide Symptom Possible Cause Remedy Intermittent spray spectrum that drops to zero periodically or randomly Drops form on emitte
71. i 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 C pericolo di esplosioni a causa del tipo di gas o liquido utilizzato E presente una radiazione ionizzante Seguire le istruzioni del manuale per lavorare con una maggiore sicurezza Non tenere le mani o le dita vicino Ar A VARIAN 1of4 Norme di Sicurezza Per lavorare in modo sicuro sullo strumento Vi consigliamo si adottare le seguenti procedure Verificare periodicamente che non ci siano perdite sulle linee e sui raccordi pneumatici Evitare che le linee dei gas vengano piegate o forate Le linee vanno posizionate in modo tale da non essere calpestate e lontane da sorgenti o troppo calde o troppo fredde I solventi organici vanno conservati in armadi speciali antiincendio ventilati e con indicazioni chiare sul contenuto di materiali tossici e o infiammabili Non accumulare i solventi utilizzati Adottare un programma regolare di smaltimento ma mai nelle acque di scarico AVVERTENZA Questo strum
72. i ete qe nete p tea iene o e ee i Hr e a 14 Installingithe Quartz Tubes iieri ep rii tin iris 15 APGI Tro bleshooting srin etta aiei edanean adaa aa aad aaea nf Eat ant a med rene te Are nr tx eb aded 17 Comparison of ESI and APCI Parameters sisi 17 APGESpate Paritaria 19 03 914981 00 3 1 03 914981 00 3 Overview of APCI Introduction Basic Principles Atmospheric Pressure Chemical lonization 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 Optimization of APCI also requires an understanding of the relationship between the mobile phase solvents and the chemistry in the ionization process Unlike ESI in which ions are extracted from droplets of mobile phase APCI is a gas phase reaction between a reagent ion typically from the mobile phase and a neutral molecule of the analyte This difference alters the APCI conditions for reversed phase chromatography and opens APCI to other modes of chromatography such as normal phase and in turn to modified sample preparation schemes APCI and ESI are complementary but significantly different in terms of setup and optimization When the appropriate criteria for APCI have been met chemical ionization
73. ial t xico y inflamable No acumule disolventes inservibles Deseche todo el material inservible a trav s de un programa especial de desechos y no a trav s del sistema convencional NOTA Este instrumento ha sido testado bajo las normas de la Directiva EMC seg n requerimientos de la Marca CE de la Uni n Europea Por lo tanto este equipo puede ser sensible a niveles de radiaciones interferencias 6 frecuencias que no est n incluidas dentro de los l mites testados 4 Este instrumento est dise ado para an lisis cromatogr fico de muestras preparadas LAN ATENCI N P g prep apropiadamente Debe ser operado usando gases y 6 disolventes apropiados y con unos niveles m ximos de presi n flujos y temperaturas seg n se describe en este manual A ATENCI N El Usuario tiene la obligaci n de informar al Servicio T cnico de Varian cuando el instrumento vaya a ser empleado para an lisis de muestras peligrosas de origen biol gico radioactivo t xico antes de comenzar a realizar cualquier an lisis Peligros El ctricos Desconecte el instrumento de todos las conexiones el ctricas a la red antes de retirar los paneles para evitar la posible exposici n a peligrosos voltages Cuando sea necesario emplear una clavija el ctrica no original asegurese de colocar los cables de acuerdo con el c digo de colores y polaridades descritos en el manual y los c digos de seguridad de la red el ctrica Sustituya los fusibles fundidos
74. ian dem Kunden den Arbeitsaufwand und andere Unkosten durch mehrfache oder fortgesetzte Installationsanfor derungen berechnen Softwareprodukte Wo Software innerhalb des Rahmens eines Lizenz abkommens 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 Kun den festgelegt gilt die Garantiezeit der Allgemei nen Lieferbedingungen Varian garantiert f r solche Soft wareprodukte die mit Varian s Hardware benutzt und richtig installiert sind oder zur Ausf hrung mit anderer von Varian angegebener Hardware wie sie in der beige f gten Bedienungsanleitung beschrieben ist da sie im wesentlichen frei von solchen Defekten sind die Fehler bei der Ausf hrung der jeweiligen Programmieran weisungen verursachen Varian garantiert jedoch keine ununterbrochene oder fehlerfreie Arbeitsweise Abhilfen Die einzige und ausschlieBliche Abhilfe in der Hardware garantie wird die Reparatur der Instrumentst rungen sein die sich nach Varian s Ansicht auf Defekte in den Originalteilen oder bei der Herstellung zur ckf hren l t oder nach Varian s Wahl der Austausch der entspre chenden defekten Teile oder die Erstattung eines fairen Teils des Kaufpreises des Instruments oder Zubeh rs vorausgesetzt da sich Varian alternativ daf r entschei det Reparatur oder Aus
75. in 872 833 Flow e Ready B 0 0 nL min 158 7 nL min 92 0 116 3 Load Q No Fault 5 0 0 nL min N A 00 100 2 Flow Total Flow N A System Setup HideKeypad Elution Status Not Ready RARES PERLES Activity Gradient Program Completed Pressure amp Flow bA Instrument 1 Nov 11 13 13 22 Single Sample Completed Resume will continue the Open SampleList 36 Item Description Composition Display The B composition When a method is running the program for the composition is also overlaid on the display so that the composition traces out the progress along the programmed composition as the method runs Pressure Display The pressure traces of the A and B pumps Time Event Markers will appear on this display at different stages of 216 LC equilibration run preparation and gradient running Flow Display The flow traces of the A and B pump Time Event markers will be appear on the display at different stages of 216 LC equilibration run preparation and gradient running GLP Dialog Box 216 1C 44 IPAddress 10 190 79 127 Manufacturer Proxeon Biosystems A S Model EASY nLC HPLC Serial Number LC 000185 Software Version HPLC 2 4 2921 04 03 2008 13 10 Sample Loop Volume 20 00 uL Injection Needle Volume 10 25 uL Cooler Actual Temperature 7 0 C Pressure Ranges PreColumn Equilibration A 0 2 137 1 bar B 0 1 0 0 bar Analytical Column Equilibration A 62 8 190 9 bar B 0 1 0 0 bar
76. ing 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 QUALITY SYSTEM Ie 19 9001 Our overriding aim is to be that partner p E RTF se D 03 914451 00 4 1 of 1 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
77. ing on whether Status sample is eluting onto the analytical column Activity Shows the different activities of the 216 LC such as Sample Pickup Precolumn Equilibration Analytical Column Equilibration and Run Gradient Some of these activities are printed on the Flow and Pressure plots during a run Button Bar System Setup Hide Keypad Composition amp Pressure amp Flow Y Item Description Hide Keypad Toggles between hiding and showing the keypad Used to View Keypad hide or display the keypad in order to enlarge or reduce the size of the Pressure Flow and composition plots GLP Displays the GLP dialog box which documents software and hardware information obtained from the instrument System Setup Allows the user to switch to a different AutoSampler tray NOTE Be sure to make sure that the AutoSampler tray installed on the 216 LC matches this selection Resume Plot Resume the plot after a run has finished Display mode This drop down box provides 4 options for configuring the selection display Flow amp Pressure amp Composition Pressure amp Flow Composition amp Pressure amp Flow Composition 34 AutoSampler Plate Display 2 101000 600000 900000 VOOCOOO Double click a well vial position to open the Inject Single Sample dialog box to inject a single sample Item Description Red fill Indicates wells vials listed in the active SampleList that have not yet been sampled Green
78. is step Add a step at the end of the program Insert a step before the selected step Delete the selected step or steps Preserve the aspect of the program by scaling the steps to a new end time This is limited by the 1 second resolution of the time program Insert a specific amount of time in the program at a specific time useful to extend a step in the middle of a program Remove a specific amount of time from the program at a specific time This is not allowed to span multiple steps The editor computes and displays the total volume of each solvent required In most cases the volumes are only a few microliters However to work above 1 uL min for hours the volumes required for a single gradient may exceed the capacity of the syringe pumps If the A or B volumes exceed 135 uL the affected volume is flagged in red a message is displayed and you cannot save the method until after you decrease the solvent usage Equilibration Programs Pre Column Re E quilibration Analytical Column Re E quilibration Maximum Pressure Volume uL 150 Volume uL 35 Phase at en Flow uL min 5 00 Flow uL min 0 30 i Item Description Pre Column Re Equilibration Volume uL Flow uL min 0 to 137 0 uL Total volume to flow though the column during the equilibration phase Specify a 0 volume to omit this phase 0 01 to 100 0 uL min Flow rate to use during equilibration Note that Pmax may be reached at a flow much low
79. is stops a run in progress 32 Pump Status Pump B S Pump Status Flow Setpoint Actual Flow Pressure bar Available Volume uL 0 0 nL min 5 2 nL min 0 1 95 8 0 0 nL min 4 4 nL min 0 2 83 0 0 0 nL min N A 0 0 100 2 Item Description Pump Designates the pump for each line of status A B S Flow Setpoint Flow that has been designated from the Method or Sample List for each pump The flow rate will switch between nL min and uL min depending on the flow rate of the pump Actual Flow The actual flow that is pumped by each 216 LC pump The flow rate will switch between nL min and uL min depending on the flow rate of the pump Pressure The pressure of each of the pumps bars Available The remaining volume that is present in the pumps uL Volume Valve Status Valve Status Flow B Flow S Load W Flow This section shows the valve status for each of the four valves in the 216 LC system The labels 1 2 1 6 and Center shown on the valves on the Home page of the 216 LC pump correspond to the following valve states Valve Label 1 2 1 6 Center A Refill Flow Closed B Refill Flow Closed S Load Inject Closed W Flow Waste Closed 33 Elution Status and Activity Elution Status Not Ready Activity Init This section shows the different states of the 216 LC pump during sample pick up equilibration and gradient run Item Description Elution Switches between Not Ready Ready depend
80. itung will Ihnen bei der Aufstellung solcher Arbeitsbedingungen helfen die einen sicheren und wirkungsvollen Gebrauch Ihrer Ger te erm glichen Besondere berlegungen und VorsichtsmaBnahmen erscheinen in diesem Handbuch in Form von HINWEIS ACHTUNG und WARNUNG wie unten beschrieben Es ist wichtig daB Sie Ihr Ger t in bereinstimmung mit dieser Arbeitsanleitung und allen m glichen zus tzlichen Informationen von Varian betreiben Alle Fragen bez glich Sicherheit und Handhabung Ihres Ger tes richten Sie an Ihr Varian B ro HINWEIS Eine Information um einen optimalen Wirkungsgrad Ihres Instruments zu erzielen Warnungssymbol WARNUNG ELEKTRISCHER SCHLAG WARNUNG CHEMISCHE GEFAHR WARNUNG VERBRENNUNGSGEFAHR WARNUNG AUGENVERLETZUNG WARNUNG FEUERGEFAHR A WARNUNG EXPLOSIONSGEFAHR WARNUNG STRAHLUNGSQUELLE WARNUNG BEWEGTE TEILE 03 914603 81 11 Necirune Weist auf Situationen die zu m iger Beeintr chtigung und oder zu Ger tesch den f hren und auf die Vermeidung dieser Situationen hin warnune Weist auf m gliche Gefahrensituationen die zu ernsthaften Verletzungen fiihren k nnen und auf die Vermeidung dieser Situationen hin Warnungsbeschreibung Gefahrliche Spannungen bestehen innerhalb des Instruments Trennen Sie das Ger t vom Netz bevor Sie abschraubbare Paneele entfernen Gef hrliche Chemikalien k nnen vorhanden sein Vermeiden Sie jeden Kon takt besonders beim Auf
81. l components of the system should be connected to a common power supply and common ground This ground must be a true ground rather than a floating ground Non polar solvents can develop a static charge when pumped through the system All vessels that contain mobile phase including tubing and collection vessels must be grounded to dissipate static electricity Employ static measuring and static discharge devices e g air ionizers to safeguard against the buildup of static electricity Ultraviolet Radiation Liquid chromatograph detectors that use an ultraviolet light source have shielding to prevent radiation exposure to personnel For continued protection m Ensure that protective lamp covers of variable and fixed wavelength detectors are in place during operation m 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 This equipment has been tested and found to comply with the limits of a Class A computing device pursuant to part 15 of the FCC Rules These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment This equipment generates uses and can radiate radio frequency energy and if not installed and used in accordance
82. ld result in serious injury and how to avoid these situations Hazardous voltages are present inside instrument Disconnect from main power before removing screw attached panels Hazardous chemicals may be present Avoid contact especially when replenishing reservoirs Use proper eye and skin protection Very hot or cryogenically cold surfaces may be exposed Use proper skin protection Eye damage could occur either from flying particles chemicals or UV radiation Use proper eye and face protection The potential for fire may be present Follow manual instructions for safe operation The potential for explosion may exist because of type of gas or liquid used Ionizing radiation source is present Follow manual instructions for safe operation Keep hands and fingers away Ar A VARIAN 1of4 General Safety Precautions Follow these safety practices to ensure safe equipment operation Perform periodic leak checks on all supply lines and pneumatic plumbing Do not allow gas lines to become kinked or punctured Place lines away from foot traffic and extreme heat or cold Store organic solvents in fireproof vented and clearly labeled cabinets so they are easily identified as toxic and or flammable materials Do not accumulate waste solvents Dispose of such materials through a regulated disposal program and not through municipal sewage lines NOTICE This instrument has been tested per applicable requireme
83. lect Inst setup others from the Tools menu F Tune init Scan From Qui Macros User pml NE Pml Editor Fe IGO ma Plot tic readbacks vaporizing Sas 220 00 pel Analog output of Capillary es en ES MSMS Breakdown A eii m Bakeout system Nea So Overnight Standby Troubleshooting Positive Inst setup others Instrument Setups Others V Warning Please perform these operations carefully Setup coarse resolution E Quad 1 C Quad3 C Both Others C Zero the collision cell pressure Zero the APCI Needle current C RF generator optimize Dip Execute Close 5 After the routine is done plug the corona high voltage connector into the socket marked Needle Voltage 6 Close and latch the chamber WARNING The Source must be vented to an external fume hood INHALATI ON or an external exhaust Failure to properly vent the ion HAZARD source can result in hazardous vapors being released into the laboratory Atmospheric Pressure Chemical lonization APCI Daily Startup and Shutdown Tuning Startup 1 Setthe vaporizer and drying gas temperatures 2 Click the spray icon DI 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 4 After waiting a few minutes for the temperatures to stabilize the APCI is ready to use Shutdown 1 Turn off the LC pump flow A
84. licita comprese senz intento limitativo le garanzie di commerciabilit ed idoneit a scopi impieghi od applicazioni specifici nonch tutti gli altri obblighi o responsabilit della Varian a meno che le altre garanzie obblighi o responsabilit in parola non siano stati accettati per iscritto dalla Varian Limitazione degli interventi e delle responsabilit Quelli qui contemplati sono gli unici ed esclusivi interventi cui ha diritto il Cliente In nessun caso la Varian sar responsabile per danni indiretti o consequenziali mancata disponibilit perdita di produzione o altre perdite subite 1of1 ap AS VARIAN 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 garant a de calidad en el dise o desarrollo fabricaci n instalaci n mantenimiento y asistencia t cnica de productos Se han convertido en el banco de pruebas de garant a de calidad a nivel mundial y miden el grado de compromiso de una empresa con la calidad as como el alcance de sus sistemas de calidad Diversas organizaciones mundiales como la British Standards Institution BSD proporcionan expertos titulados de probada objetividad para investigar procedimientos de calidad desarrollo de productos procesos de fabricaci n y programas de servicio al cliente Varian Inc Analytical Instru
85. llow the pump pressure to decrease and stabilize so flow into the interface stops 2 Click the spray icon to turn off the gases and heaters The heaters switch off immediately and after a few seconds the gases switch off The heaters will continue to cool 3 Check that the mobile phase is no longer flowing before opening the spray chamber Tune and mass axis calibrate of the 1200L mass spectrometer using the Electrospray lonization ESI chamber Refer to the Tuning section of the 1200L manual APCI Mobile Phase Selection Most common HPLC mobile phases are ideal for LC MS Normal phase solvents such as dichloromethane hexane and toluene while unsuitable for ESI are well suited to APCI APCI can handle highly aqueous mobile phase compositions however you should use mobile phase additives with caution Because APCI is a gas phase ionization method and because mobile phase constituents are present in large excess compared to the sample severe quenching of the analyte signal can occur Particularly troublesome are additives such as formate and acetate in negative mode APCI APCI usually uses a higher flow rate than ESI HPLC flow rates for APCI should be between 0 1 to 2 0 mL min with optimum performance realized between 0 5 and 1 0 mL min supporting the most common 2 1 and 4 6 mm ID HPLC columns When operating at higher or lower flow rates the temperature of the APCI vaporizer should be raised or lowered appropriately 03 914981
86. mark of Quality outre les contacts directs que nous tablissons avec chacun de nos clients Nos produits et nos proc d s sont con us pour r pondre vos attentes Nous n ignorons pas que vous recherchez plus que des processus volu s et un savoir faire d exception dans le domaine des applications Vous souhaitez conjuguer vos forces avec un partenaire s tant engag offrir une qualit une fiabilit et une valeur optimales au moment o il faut et quand il faut QUALITY SYSTEM IO9001 Notre principal objectif devenir votre partenaire AAA 03 914451 82 4 1of1 Garantie des instruments d analyse Varian Inc Mat riel Les instruments d analyse vendus par Varian Inc sont garantis exempts de d fauts de mati re et de fabrication pour les p riodes sp cifi es et conform ment aux conditions mentionn es sur le recto du devis ou aux termes de tout autre accord crit intervenu entre Varian et le client La p riode de garantie commence compter de la date de livraison de Varian au client d origine Cependant lorsque le client a acquitt les frais d installation ou que celle ci est inclue dans le prix d achat la p riode de garantie commence compter de l ach vement de l installation Si le client pr voit le d but de l installation au del de 30 jours apr s la livraison ou si ledit retard est d l inaptitude du client mettre disposition les installations ou services ou au non respect des inst
87. ment to display these parameters Set the Emitter Voltage Spray Shield Voltage Drying Gas Pressure and Drying Gas Temperature for a specific segment Method Active Segment Module Attributes Optimization Plots Method Segment MW Detector On Scan Type Full v ScanMode Standard v Defaults m Syringe Pump On General Parameters Ionization Control Nanospray lonization Parameters Full Scan Parameters Emitter Voltage Positive volts Negative volts Drying Gas Pressure psi T Spray Shield Voltage IT Drying Gas Temperature G Positive volts Negative volts Figure 16 25 Method Builder Click MS Acquisition Method in the tree to display the MS parameters Method1 Method Notes ET 500 MS Mass Spec Address 56 ET 500 MS Mass Spec Control Y MS Acquisition Method Select Nanospray in the Instrument Configuration menu Enter suitable values in the Nanospray lonization Parameters tab Refer to Figure 17 to set individual segment parameters for Nanospray in the Method Editor li Method Builder Method1 Uh File Edt View Window Heb 5x asas alba lela Sr 14 4 gt pI RE 3810 ED Method Notes pi ia Acquisition Data Type TubeDOS ET 500 M5 Mass Spec Address 56 7 c C Ceod Profile T TubcDDS Method E 500 95 Mass Spec Contro DT MS Acquistion Method E Channel 1 145 Data f standard MS Reports Print Options
88. ments fue registrada en 1992 con la norma m s exhaustiva de la serie ISO 9000 la ISO 9001 La certificaci n por la norma ISO 9001 significa que todas las etapas de nuestro sistema de calidad como el desarrollo del producto la fabricaci n las pruebas finales la expedici n as como los suministros y recambios han sido examinados rigurosamente respecto a las normas m s exigentes reconocidas internacionalmente Significa que nos comprometemos a mantener un nivel de calidad con el que podr siempre contar hoy y en el futuro Il nostro Sistema di Qualit ha ottenuto la certificazione ISO 9001 col numero FM21797 Los sistemas de calidad que nos valieron la certificaci n ISO 9001 representan beneficios directos para nuestros clientes haremos llegar nuestros aparatos m s r pidamente que nunca Podemos cumplir con pedidos urgentes a n m s deprisa Atenderemos sus pedidos de forma r pida y completa Aplicamos un sistema de retorno de informaci n permanente con nuestros clientes siempre somos conscientes de sus necesidades actuales o futuras Hemos mejorado la productividad de nuestros clientes disminuyendo el ndice de defectos a la mitad y acortando el tiempo de respuesta del servicio de mantenimiento Hemos integrado sistemas de mejora continuada en nuestra organizaci n de forma que podremos obtener niveles de calidad a n superiores en un futuro Estamos integrando los requerimientos GLP en nuestros productos
89. mic insulating washer 03 937323 01 into the cutout on the vaporizer covering the top of the heater Gently press on the washer to seat it in the cutout 3 Take the new quartz tube 03 937327 01 and place the O ring 03 930109 06 over the end The quartz tube should be barely protruding from the O ring for this step 4 Carefully lower the new quartz tube into the heating coil of the vaporizer The O ring on the quartz tube will be resting on the insulating washer when the quartz tube is properly installed If the quartz tube does not go in all the way GENTLY rock the insulating washer and or the quartz tube with gentle pressure taking care not to break the quartz tube DO NOT FORCE THE QUARTZ TUBE INTO THE HEATING COIL If the quartz tube snags the heating coil and damages it the vaporizer assembly must be replaced Once the quartz tube is in the heating coil gently press on the end of the tube to push it slightly below the O ring Ceramic Insulating Washer White Quartz Tube below surface of O ring O ring A D Proper Depth of Quartz Tube in O ring Atmospheric Pressure Chemical lonization 15 16 15 16 Open the spray chamber keeping a finger on the quartz tube through Step 7 so it doesn t fall out 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 Replace the compression fitting and tighten finger tigh
90. n infiammabili m Installare un aspiratore in uscita m Posizionare la presa d aria in modo che le vibrazioni e il movimento dell aria non disturbino il rivelatore m Eseguire verifiche periodiche per garantire un funzionamento corretto m Garantire una buona ventilazione nel laboratorio Rivelatori a Sorgente Radioattiva m Leggere e rispettare tutte gli avvisi di NOTA CAUTELA e ATTENZIONE riportati nel manuale del rivelatore ECD al Ni m Eseguire tutti i test di contaminazione radioattiva rimovibile descritti nel manuale dell ECD al Ni m Rispettare tutte le procedure e le scadenze di verifica per eventuali perdite 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 sotto pressione la pompa pu liberare liquidi tossici e o volatili molto pericolosi m E opportuno adottare un sistema di protezione del viso quando si inietta il campione o si esegue una manutenzione routinaria del sistema 03 914603 83 11 m Non smontare mai una linea del solvente od una valv
91. nsitivity is lost or if excessive peak tailing occurs Clean the drying gas spray shield the vacuum capillary the corona needle and the quartz vaporizer tube NOTE The quartz vaporizer tube may look dirty and the performance may not be affected Replace it only if performance degrades Cleaning the Spray Shield 1 Remove the spray shield by gently rotating it off the mounting posts 2 Wipe it with methanol or if needed scrubbing with an aluminum oxide powder water slurry Rinse with distilled water and then a methanol rinse Replace the spray shield by engaging one detent on the shield with one of the mounting posts and then using a gentle rotating motion to engage the other 5 Check that the capillary is visible and centered in the hole Cleaning the Vacuum Capillary You can rinse the outer end of the capillary without venting the system Using a wash bottle spray a small amounts of water or methanol into capillary You can remove the spray shield If more extensive cleaning of the inside of the capillary is required the system must be vented the capillary removed Place it inside a graduated cylinder in an ultrasonic bath and clean it Atmospheric Pressure Chemical lonization 11 Cleaning the Corona Needle Wipe the corona needle with methanol If the deposits cannot be easily removed replace the needle as follows Cutaway View of APCI Chamber Replacing and Aligning the Corona Needle Replace the corona needl
92. nte 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 unit delle serie solo in base alla loro disponibilit 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 V sendorf bei Wien Tel 43 1 699 9669 Benelux Bergen Op Zoom Tel 31 164 282 800 Brazil and Latin America S S o 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 4 of 4 France Les Ulis C dex 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 King
93. nts of EMC Directive as required to carry the European Union CE Mark As such this equipment may be susceptible to radiation interference levels or frequencies which are not within the tested limits This instrument is designed for chromatographic analysis of appropriately prepared samples It A warnine must be operated using appropriate gases and or solvents and within specified maximum ranges for pressure flows and temperatures as described in this manual If the equipment is used in a manner not specified by the manufacturer the protection provided by the equipment may be impaired the instrument has been used for the analysis of hazardous biological radioactive or toxic It is the responsibility of the Customer to inform Varian Customer Support Representatives if WARNING 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 original power cord plug make sure the replacement cord adheres to the color coding and polarity described in the manual and all local building safety codes Replace blown fuses with fuses of the size and rating stipulated on the fuse panel or in the manual Replace faulty or frayed power cords immediately with the same type and rating Make s
94. oa NE Inject the sample 15 Columns There are at least two types of columns that can be used These columns differ in their OD and how they are connected Connecting Columns 1 32 in OD PEEK These are the simplest to use 1 Connect the inlet of the column to the 1 32 in nut on the tee 2 Connect the outlet of the column to the 1 32 in nut on the inlet of the conductive union To Waste Tee Pump a Flow gt Column Conductive Union Figure 10 Connecting Columns 360 um OD Fused Silica A sleeve is used to adapt the column to the 1 32 in nuts 1 Place a piece of 1 32 in sleeve on each end of the column 2 Insert the sleeve end of the column into the nut then into the ferrule making sure the sleeve and column extend through the ferrule a few millimeters To minimize the connection volume the sleeve must be bottomed out in the union and the column must be flush with the end of the sleeve 3 Repeat step 2 on each end of the column Ensure that the column inlet connects to the valve and that the column outlet connects to the conductive union To Waste Pump Flow j Trapping Column Conductive Union Figure 11 NOTE If the nut is tightened without tubing or a sleeve inside the ferrule the ferrule may become damaged and must be replaced as the hole becomes too small for the sleeve 16 Optimizing Operating Parameters 1 Place the conductive union into the union holder on the nESI interf
95. odotto un costante miglioramento nella nostra struttura organizzativa in modo da poter conseguire in futuro livelli qualitativi ancor pi elevati Stiamo adeguando i nostri prodotti e servizi agli standard GLP per poter aiutare 1 clienti a soddisfare i requisiti di conformit posti loro dagli enti normativi Ma l omologazione ISO 9001 non tutto Per quanto ci riguarda la qualit viene definita dai nostri clienti noi siamo soddisfatti solo se lo il cliente Ci adoperiamo al massimo per comprendere le esigenze del cliente ricorrendo ad indagini di societ private gruppi di utenti associazioni di consumatori e con il nostro programma di risposta Hallmark of Quality il marchio di garanzia di qualit 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 pi 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 affidabilit e valore in modo tempestivo e costante QUALITY SYSTEM ISI 9001 Quel partner vogliamo essere noi cz RT rr eo 03 914451 83 4 1 of 1 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
96. oflow HPLC system see Using a Column and Nanoflow LC on page 15 Basic Operation Overview The nESI lon Source uses an emitter to introduce samples to the MS The camera has a magnifying lens which is focused on the spray The image is displayed on the computer monitor allowing you to optimize the spray while changing the parameters The nESI lon Source has the following features i USB Cable for Camera 4 Camera e 9 4 Lens Side to Side Camera Adjustment Lens Focus Back to Front Camera Adjustment Chamber Latch Chamber Latch Chamber Door Handle Up and Down Emitter Adjustment Side to Side Emitter Adjustment In and Out Emitter Adjustment Figure 1 The nESI lon Source has the following connections To Needle Voltage Socket er API Housing Socket Figure 2 Magnets hold the spray chamber door in place and it can be raised or removed The following shows the emitter pulled out and the spray chamber door open slightly Figure 3 Installing the nESI lon Source Installing the nESI lon Source WARNING BURN HAZARD Source parts may become hot during operation Use caution when installing or removing the API Source Nerurion The lon Source is heavy and delicate Handle it carefully using both hands WARNING INHALATION HAZARD You must vent the source to an external fume hood or an external exhaust Failure to do so may release hazardous vapors NOTE You must tune th
97. ola quando il sistema sotto pressione Fermare prima la pompa ed aspettare che la pressione scenda a zero m Usare dei contenitori per solventi infrangibili ed in grado di lavorare a 50 60 psi m Quando i contenitori sono sotto pressione usare una protezione esterna m Leggere e rispettare tutti gli avvisi di NOTA CAUTELA e ATTENZIONE Cromatografia Flash L operatore deve conoscere le propriet fisico chimiche delle componenti della fase mobile I solventi non vanno messi in contatto diretto con il tubo di erogazione in poliuretano dal momento che alcuni solventi possono causare indebolimento e perdite con possibili scoppi Tutte le componenti del sistema vanno collegate ad una fonte di alimentazione e ad una messa a terra comuni E meglio che per quest ultima venga utilizzata una spina con polo di terra I solventi non polar possono sviluppare una carica statica quando vengono pompati attraverso il sistema Tutti i recipienti che contengono la fase mobile inclusi 1 tubi e i recipienti di raccolta devono avere una messa a terra per disperdere l elettricit statica Vanno utilizzati dispositivi di misurazione e scarico ad esempio ionizzatori d aria per evitare l aumento di elettricit 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
98. on check the seating of the parts and tighten the nut holding the emitter in the union e Asthe syringe plunger wears it will leak As a result liquid will accumulate in the barrel of the syringe behind the plunger and the visible spray in the camera image will decrease Compensate for small leaks by increasing the flow rate Replace the syringe if the leak is larger 13 Parameters for the nESI lon Source The following parameters are suggested as a starting place for the ionization of most samples Optimize the parameters for your sample These parameters are applicable for both the 300 Quadrupole LC MS and the 500 MS IT LC MS Table 1 Default Method Parameters for the 500 MS and the 300 Series LC MS Parameter Starting Value Emitter Voltage 2000V Shield 300V Drying Gas Pressure 12 psi Drying Gas Temperature 250 C Spray Chamber Temperature 35 C Operating Hints When optimizing the voltage after installing a new emitter begin at the lowest voltage that produces a spray Operating at too high a voltage may damage the tip of the emitter As the emitter ages increase the voltage to maintain the spray This may be caused by erosion of the sharp point at the tip of the emitter deposits on the tip of the emitter or both After the voltage is optimized the appearance of the spray plume depends greatly on the composition of the mobile phase Mobile phases with a high percentage of methanol or a
99. ontinue Anyway Setting Up the Camera Software Double click on the icon on the desktop to start the software Select Option_Settings from the menu Click Advanced Under Rotation on the Other tab select Clockwise_90 Under ALC mode on the Gain Shutter tab select ALC_FullAuto AGC ON Click Save and then click Yes to Save as Initial Setting for this Camera Type This retains these settings when the software is restarted QI Qv des OURS at Installing an Online Emitter for Infusion Analysis Successful nanospray operation depends on the performance of the emitter The Varian nanospray system accommodates many types of emitters fused silica metal polymer tipped emitters and emitters integral to the column While the following information is specific for the stainless steel emitters which are available from Varian it also applies to the other emitter types Infusing samples with a syringe pump is a good technique when a sufficient volume of sample is available and a chromatographic separation is not needed Having the sample constantly introduced is helpful for optimizing nanospray conditions The syringe drive moves the syringe plunger pushing the liquid out of the syringe through the connecting tubing and out the emitter Typical flow rates are 100 500 nL min 0 1 to 0 5 uL min or higher Assembling the Syringe and Emitter 1 Draw the sample into the syringe 2 Connect the syringe to the luer adapter and the rest of the
100. ow bypasses the analytical column during this step This allows sample volumes that are compatible with conventional sample handling techniques typically 1 10 pL to be used Second because the sample is loaded onto the trapping column at weak solvent strength the sample is concentrated in a very narrow band at the top of the trapping column A solvent gradient elutes the individual peptides through the analytical column and out the emitter This produces very sharp peaks even from 10 uL injections Typical flow rates are 200 400 nL min for a 75 um ID column The exact rate depends on column length and the particle size At the beginning of each run the 216 LC method has parameters that automatically re equilibrate the columns to the initial solvent composition The valves are built in to the 216 LC and are automatically switched while the method is running To install or change a column the connections to the 216 LC are to the ends of the two PEEKsil tubes The pump flow the gray tube connects to the inlet of the trapping column and the connection back to the waste valve the black tube connects to the side port of the tee of the column assembly The following is a brief overview of the process detailed information follows Connect the column assembly between the 216 LC and the emitter Verify the flow and check for leaks Determine the equilibration flow rates Determine emitter voltages Build the workstation method Qu agb d
101. por otros fabricantes consumibles o art culos de duraci n de vida limitada como son entre otros filtros elementos de vidrio pilotos l mparas diafragmas columnas fusibles papel y tinta de gr ficos nebulizadores c lulas de flujo pistones cierres juntas v lvulas quemadores tubos de muestras inserciones de sondas cabezales de impresi n tubos de vidrio juntas de tubo dispositivos de temperatura variable l neas de transferencia disquetes cintas magn ticas multiplicadores de electrones filamentos juntas de vac o soportes y todos los componentes en contacto con muestras y partes m viles Esta garant a no tendr efecto en los casos de accidente abuso alteraci n utilizaci n incorrecta negligencia rotura mantenimiento o uso inadecuados modificaciones inadecuadas o no autorizadas uso de la fuerza uso en un entorno inadecuado funcionamiento con una alimentaci n defectuosa o el uso con medios inadecuados Es necesario tomar las precauciones adecuadas para evitar riesgos Las garant as de los productos de software de Varian sustituyen y excluyen cualquier otra garant a impl cita o expl cita incluidas pero sin limitaci n las garant as de comerciabilidad adecuaci n a un fin uso o aplicaci n en particular y todas las dem s obligaciones y responsabilidades por parte de Varian a no ser que estas garant as obligaciones y responsabilidades sean otorgadas expresamente y por escrito por Varian
102. r end when the spray stops Bubbles in mobile phase 1 Degas mobile phase prime pump 2 Decrease drying gas temperature 3 Increase emitter voltage 4 Wait for the bubbles to be flushed No peaks in chromatogram Sample not picked up from vial 1 Refill A S wash bottle and re prime the S pump 2 Run sample pickup test script No spectrum and no visible spray System not pressurized Pumps not running Plugged emitter Syringe leaks Run maintenance scripts to check for proper pump function and pressure Replace emitter Check all unions and autosampler syringe replace if necessary Unsteady flow in pump graphs May show periodic oscillations in the actual flow Air in one of the pumps Check solvent levels Run flush air script Pressure lower than expected or not increase proportionally with increasing flow Leak in flow path Find leaking fitting reseat tubing and tighten fitting Pump does not prime Flush air test does not pass Level in solvent bottle too low Fill bottle Prime purge pump Pump does not prime Flush air test does not pass Malfunctioning check valve Replace check valve Pressure higher than expected or not increase proportionally with increasing flow Blockage in flow path Damaged fused silica tubing Replace damaged tubing Install new filter element Install new column or emitter 20 3
103. r to point the tip of the emitter to the upper half of the spray shield hole The following picture of a view through the front window has a star in the correct position Spray shield View through front window Figure 8 12 Setting Workstation Parameters and Optimizing Emitter Conditions 1 Verify that the syringe volume setting corresponds to the syringe in use e 500 MS Module Attributes tab e 320 MS Instrument Parameters dialog Syringe tab 2 Verify that the purge rate is set to 10 uL min or less ZN caution Using a purge flow rate higher than 10 uL min can break the syringe 3 Set the flow rate to 0 3 uL min and adjust as needed 4 Start the syringe pump 5 Verify the flow and check for leaks 6 After the emitter flows for a few minutes look for small drops of solvent forming at connections If any leaks are seen check that the sleeve extends through the ferrule and tighten that fitting a little more into the union 7 Optimize the emitter voltage observing both the mass spectrum and the camera image If no spray is seen there may be a leak of back connection Reseat connections and check for leaks Suggestions e After refilling the syringe flush the sample through the connecting tubing to remove any bubbles by purging for a few seconds e Check for liquid coming out the emitter tip before turning on the high voltage If liquid emerges between the emitter and the sleeve after the conductive uni
104. rian no garantiza la utilizaci n ininterrumpida o libre de errores Recursos El nico y exclusivo recurso en cuanto a hardware bajo garant a ser reparar los defectos del aparato que en opini n de Varian sean claramente imputables a defectos de los materiales originales o de fabricaci n 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 per odo de garant a no prolongan el per odo de garant a original 03 914412 84 2 Las reparaciones o sustituciones en per odo de garant a se efectuar n a criterio exclusivo de Varian enviando un representante de servicio posventa a la instalaci n o autorizando al cliente a reexpedir el componente o aparato defectuoso a Varian o a un servicio de reparaci n designado El cliente ser responsable sobre p rdidas o da os de transporte y pagar los costes de dicho transporte Varian reexpedir el componente o aparato a portes pagados y con seguro de transporte Las demandas por da os o p rdidas deber n ser gestionadas por el cliente Para corregir anomal as de funcionamiento de software Varian editar revisiones de software siempre y cuando stas est n disponibles y cuando en opini n de Varian este sea el remedio mas eficaz Limitaci n de garant a Esta garant a no cubre software provisto por el cliente equipos y software garantizados
105. rian pour toute question commerciale ou de service d assistance la client le ou pour passer commande de pi ces et de fournitures Argentina Buenos Aires Tel 54 11 4 783 5306 Australia Mulgrave Victoria Tel 61 3 9566 1134 Austria V sendorf bei Wien Tel 43 1 699 9669 Benelux Bergen Op Zoom Tel 31 164 282 800 Brazil and Latin America S S o 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 4 of 4 France Les Ulis C dex 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 Ar A VARIAN www varianinc com 03 914603 82 11 Informazioni sulla Sicurezza Instruzioni per Uso Questo manuale ha lo scopo di aiu
106. rst die Pumpe an und lassen Sie den Druck auf Null abfallen m Benutzen Sie splittersichere Reservoirs die f r einen Druck von 3 4 bis 4 1 bar ausgelegt sind m Halten Sie die Reservoirverkleidung geschlossen wenn die Reservoirs unter Druck stehen m 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 L sungsmittel mit den Zuf hrungsleitungen aus Polyurethan da einige L sungsmittel das Material der Leitungen schw chen und damit Undichtigkeiten oder Br che hervorrufen k nnen 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 L sungsmittel k nnen sich beim Pumpen durch das System statisch aufladen Alle Gef e die mobile Phase enthalten einschlieBlich Leitungen und Sammelgef Be m ssen zur Ableitung elektro statischer Aufladungen geerdet sein Setzen Sie Ger te zur Messung und Ableitung elektrostatischer Aufladungen z B Ger te zur Luftionisierung als Ma nahmen gegen den Aufbau statischer Elektrizit t ein Ultraviolette Strahlung Detektoren in Liquidchromatographen die eine ultraviolette Lichtquelle benutzen besitzen eine
107. rt Format 39 216 LC Pump Program Window E ZB in fan Add 1 0 1000 Insert Z gt Delete 4 35 Scale Run Time 5 108 00 49 51 amp 11900 25 75 AgdRunTme 7 12540 1 0 i 100 2000 Subtract Run Time 8 14810 0 100 2000 m Total Volumes Required By This Program 9 15050 100 0 1000 Volume A 146 89 uL Volume B 99 79 uL Pre Column Re E quilibration Analytical Column Re E quilibration gt Maximum Pressure Volume uL 150 Verus 35 Pressure bar 300 Flow ulmin 500 Flow ul min 0 30 l n Solvent Flow Flow Composition Time Program Den A nd foin a 1000 Insert Delete Scale Run Time Add Run Time 2000 Subtract Run Time 2000 Total Volumes Required By This Program 1000 Volume 146 89 uL Volume B 99 79 uL Item Description Time Time program point in minutes seconds The maximum number of steps is 100 and the maximum time is 1440 minutes A The value of this field is calculated automatically from B B Enter the desired B value in increments of 1 The pump will ramp linearly to the specified composition from 40 Flow Add Insert Delete Scale Run Time Add Run Time Subtract Run Time Total Volumes Required By This Program the last specified time and value before this step Enter the desired flow in nL min The pump ramps linearly to the specified flow from the last specified time and value before th
108. ructions de pr installation de Varian ou la suite desdites n gligences du client la p riode de garantie commence le 31 me jour compter de la date de livraison De plus Varian fera supporter au client tout frais de main d oeuvre et autres co ts r sultant de multiples appels t l phoniques 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 limit e aux termes dudit accord En l absence d accord de licence et sauf accord crit sur tout autre p riode de garantie entre Varian et le client la p riode de garantie est telle que sp cifi e sur le recto du devis de Varian Sous r serve de leur installation et de leur utilisation correcte sur le mat riel Varian ou tout autre mat riel tel que sp cifi Varian garantie le fonctionnement tel que d crit dans le manuel d utilisation fourni avec le mat riel et l absence de d fauts entra nant l impossibilit d ex cuter des instructions de programmation respectives Toutefois Varian ne garantit pas un fonctionnement sans interruption et sans erreurs Recours Le seul et unique recours relatif la garantie du mat riel se limite la r paration suite un mauvais fonctionnement de l instrument qui de l avis de Varian est d des d fauts des pi ces d origine ou de la fabrication ou la discr tion de Varian au remplacement des pi ces d fectue
109. rument wurde nach den zutreffenden Vorschriften der EMC Direktive getestet die zum F hren des CE Zeichens der Europ ischen Union berechtigen Dieses Ger t kann an sich auf Strahlungs St rpegel oder Frequenzen auBerhalb der getesteten Grenzen reagieren dacht Es muf mit geeigneten Gasen und oder L sungsmitteln und innerhalb der im Handbuch Dies Instrument ist f r chromatographische Analysen entsprechend pr parierter Proben ge WARNUNG spezifizierten maximalen Werte f r Druck Fl sse und Temperaturen betrieben werden Der Kunde ist vor der Durchf hrung irgendeines Ger teservices verpflichtet den Varian WARNUNG Kundendienstvertreter zu informieren wenn das Instrument f r Analysen gef hrlicher biologischer radioaktiver oder toxischer Proben benutzt worden ist Elektrische Gefahren L sen Sie das Instrument von allen Stromquellen bevor Sie Schutzpaneele entfernen damit Sie nicht mit po tentiell gef hrlichen Spannungen in Ber hrung kommen Wenn ein Nicht Original Netzkabelstecker benutzt werden mu mu das Austauschkabel die im Handbuch beschriebene Farbcodierung und Polarit t beibehalten und alle rtlichen Sicherheitsvorschriften erf llen 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 daf r dab Spannungsquellen und die Netzspann
110. s d bits et des temp ratures ATTENTION a t utilis pour l analyse d chantillons biologiques dangereux radioactifs ou toxiques avant que n en soit effectu la maintenance Risques de chocs lectriques D connecter le mat riel de toute source d alimentation avant d en d monter les panneaux de protection sous peine de s exposer des tensions dangereuses En cas d utilisation d un cordon d alimentation n tant pas d origine s assurer que celui ci soit conforme la polarit et au codage des couleurs d crits dans le manuel d utilisation ainsi qu toutes les normes r gionales de s curit r gissant le secteur de la construction Remplacer les fusibles saut s par des fusibles de m me type que ceux stipul s sur le panneau des fusibles ou dans le manuel d utilisation Remplacer les cordons d alimentation d fectueux ou d nud s par des cordons d alimentation de m me type S assurer que les sources de tension et la tension de secteur correspondent la tension de fonctionnement du mat riel Bouteilles gaz comprim 2 of 4 Ranger et manipuler les bouteilles gaz comprim avec pr caution et conform ment aux normes de s curit Fixer les bouteilles gaz comprim un mur ou une structure inamovible Ranger et d placer les bouteilles gaz comprim en position verticale Avant de transporter les bouteilles gaz comprim retirer leur r gulateur Ranger les bouteilles dans un endroit bien ven
111. se sind so gestaltet da sie diese Anforderungen erf llen Wir wissen da Sie mehr als fortschrittliche Prozesse und ausgezeichnetes Anwendungswissen suchen Sie suchen einen Partner der Qualit t von Weltklasse Verl lichkeit und Nutzen f r Sie liefert p nktlich und jederzeit Unser oberstes Ziel ist f r Sie dieser Partner zu sein QUALITY SYSTEM ISIN9001 CER T IF i E B 03 914451 81 4 1 von 1 Varian Inc Analytical Instrument Garantie Hardwareprodukte Es wird garantiert da alle von Varian Inc verkauften analytischen Instrumente f r die angegebene Zeitdauer und in bereinstimmung mit den Allgemeinen Liefer bedingungen 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 Ver kaufspreis eingeschlossen ist beginnt die Garantiezeit nach der abgeschlossenen Installation Wenn der Kunde den Installationsbeginn sp ter als 30 Tage nach erfolgter Lieferung ansetzt oder wenn die Verz gerung dadurch verursacht wird daR der Kunde nicht den ausreichenden Platz oder die Ver sorgungseinrichtungen beschafft oder Varian s berechtigte Anweisungen zur Installationsvorbereitung nicht einh lt oder andere Vers umnisse des Kunden vorliegen dann beginnt die Garantiezeit am 31 Tag nach dem Versanddatum Dar ber hinaus wird Var
112. sera tenu pour responsable de tout dommage provenant de l utilisation ou en d coulant de toute impossibilit d utilisation ou de d ficit de production ou de tout autre perte y aff rent 1of1 ap AS VARIAN I sistemi di qualit della Varian Inc La serie degli standard ISO 9000 stata presentata nel 1987 a Ginevra con lo scopo di mettere ordine in un groviglio di definizioni contrastanti sulla qualit Tali standard definiscono un modello che assicura la qualit nella progettazione nello sviluppo nella fabbricazione nell installazione e nella manutenzione dei prodotti nonch 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 qualit e della validit dei sistemi di qualit da esse adottati Diverse organizzazioni internazionali come la British Standard Institution BSI dispongono d ispettori certificati e imparziali per la valutazione delle procedure di qualit dello sviluppo dei prodotti dei processi di fabbricazione e dei programmi di soddisfazione del cliente Nessuna azienda pu asserire d essere in possesso della certificazione ISO 9000 finch non dispone del marchio d approvazione concesso dai rigorosi ispettori di qualit della BSI o di altri enti di controllo riconosciuti La certificazione di conformit agli standard ISO 9000 costituisce un attestazione imparziale di terzi del
113. service Comparison of ESI and APCI Parameters PARAMETER ESI APCI Drying Gas 4L min 350 C 2L min 150 C Nebulizing Gas 60 psi 60 psi Auxiliary Gas N A 2L min 550 C Inner Needle Adjustable Fixed Needle Assembly Up Down Adjustable Fixed Needle Assembly Translation Adjustable Adjustable Needle Voltage Current 5000V 5 uA Optimum Liquid Flow Rate 200 400 uL min 0 5 1 mL min Housing Temperature 40 C 50 C Atmospheric Pressure Chemical lonization 17 APCI Spare Parts PART NUMBER DESCRIPTION Quartz Vaporizer Tube Ferrule Polyimide Ceramic Insulating Washer white These components only need replacing if they are damaged or lost Part Number Description 03 937340 01 APCI Vaporizer Compression Fitting 03 937326 01 Nebulizer Assembly Atmospheric Pressure Chemical lonization 19 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 2700 Mitchell Drive Walnut Creek CA 94598 1675 USA e Agilent Technologies 300 Series and 500 MS LC MS Mass Spectrometer Nanospray lon Source Operation Manual QUALITY SYSTEM IiS 9001 CG E R T I F 1 E D OVarian Inc 2008 Printed in U S A Part Number 395420100 1 Trademark Acknowledgments
114. t NOTE Excessive tightening can break the quartz tube The fitting is correctly tightened when gentle pressure on the end of the quartz tube cannot slide it within the vaporizer Check to see that the O ring is touching the insulating washer The quartz tube is now fixed in place and no longer needs to be held by your finger Replace the corona needle by pressing it firmly into its mount until it bottoms Close and latch the spray chamber Replace the nebulizer assembly lowering it straight down using care to first pass the nebulizing tube into the quartz tube and then to engage the alignment pins the gas lines should be on the right side Excessive rocking of the nebulizer assembly can crack the quartz tube After checking to make sure the nebulizing assembly is straight evenly tighten the two screws on top until snug Connect the large 14 pin round connector to the socket marked API Housing Connect the small 4 pin round connector to the socket marked APCI Heater Set the APCI temperature to 550 C and click on the spray icon DI to turn on the gases and heaters Allow the system to bake out for 15 minutes to remove surface contamination from the new quartz tube The APCI interface is ready to use No adjustment is necessary if the corona needle mount has not been rotated If the corona needle needs adjustment follow the procedure above 03 914981 00 3 APCI Troubleshooting If no p
115. tains solvants sont susceptibles de provoquer des faiblesses et des fuites avec risques d explosion Tous les constituants du syst me devront tre connect s une source de courant commune et une prise de terre commune Cette prise de terre devra tre fixe et non mobile Les solvants non polaires peuvent produire de l lectricit statique lorsqu ils passent au travers du syst me Les bouteilles qui contiennent la phase mobile incluant les tuyaux et les flacons de collecte de fractions doivent tre mises la terre pour liminer l lectricit statique Utiliser des appareils de mesure et de d charge d lectricit statique par exemple des ionisateurs d air pour combattre la formation d lectricit statique Radiations ultraviolettes Les d tecteurs CPL utilisant une source lumineuse ultraviolette comportent un cran destin se pr munir contre les expositions aux rayonnements Pour s assurer une protection permanente m V rifier que le couvercle de protection de la lampe des d tecteurs op rant des longueurs d onde variables et fixes soit bien en place durant le fonctionnement du mat riel m Ne pas regarder directement les cellules du d tecteur ou la source d UV Se prot ger syst matiquement les yeux lors du contr le de la source lumineuse ou des cellules par exemple au moyen de verres borosilicat s ou en polystyr ne 3 of 4 Disponibilit des pi ces de rechange La politique de Vari
116. tandard bieten auf den Sie heute und in Zukunft rechnen k n nen Unser Qualit tssystem hat die ISO 9001 Zertifikatnummer FM21797 erhalten Die Qualit tssysteme der ISO 9001 Registrierung haben f r unsere Kunden direkte Vorteile Wir k nnen Instrumente schneller denn je zu Ihnen schicken Eilbestellungen werden noch schneller durchgef hrt Wir erf llen Ihre Bestellungen p nktlich und vollst ndig Wir haben ein System kontinuierlichen Informationsr ckflusses von unseren Kunden auf gebaut wir kennen Ihre Anforderungen von heute und von morgen Wir haben Ihre Produktivit t durch Halbierung der Systemfehlerraten und durch Verk r zung unserer Reaktionszeit im Service verbessert Wir haben kontinuierliche Verbesserungen in unserer Organisationsstruktur verankert so da wir k nftig eine noch h here Qualit t erreichen k nnen Wir haben die GLP Anforderungen in unsere Produkte und Dienstleistungen eingef hrt um Ihnen bei der Erf llung Ihres beh rdlichen Abnahmeprotokolls zu helfen Die ISO 9001 Registrierung ist nicht genug F r uns wird Qualit t durch unsere Kunden de finiert Wir sind nicht zufrieden wenn Sie es nicht auch sind Wir bem hen uns die Anforderungen un serer Kunden durch unabh ngige Untersuchungen Anwendergruppen Kundenberatungsgremien und un ser Antwortprogramm G tesiegel der Qualit t zu verstehen zus tzlich zu pers nlichen Kundenkontak ten Unsere Produkte und unsere Prozes
117. tare 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 NOTA 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 Lein TO ATTENZIONE ATTENZIONE NOTA Sono informazioni utili ad ottenere le prestazioni migliori da parte dello strumento Allerta l operatore su situazioni che potrebbero causare ferite leggere e danni limitati allo strumento ed il modo di evitarle Allerta l operatore su situazioni potenzialmente pericolose che possono causare danni molto seri ed il modo di evitarle Segnali di ATTENZIONE Descrizione del Pericolo SOSTANZA CHIMICHE ATTENZIONE Pericolo di scottature ATTENZIONE JA PERICOLO PER GLI OCCHI ATTENZIONE Pericolo di incendio Y ATTENZIONE Pericolo di esplosioni ATTENZIONE Pericolo di radiazioni ATTENZIONE Parti in movimento EEE pb pl 03 914603 83 11 ATTENZIONE Nello strumento sono presenti tensioni pericolose Scollegare il cavo Pericolo di folgorazioni j A i AS a di alimentazione prima di togliere il pannello fissato con le viti ATTENZIONE zu pis ESPOSIZIONE A Possono essere presenti composti chimici pericolos
118. tausch unter Garantie verl ngert nicht die urspr ngliche Garantiezeit 03 914412 81 2 Reparatur oder Austausch unter Garantieanspr chen soll in Varian s ausschlieRlichem Ermessen entweder durch einen Serviceingenieur beim Kunden oder durch Erm chtigung des Kunden zum Einschicken des defek ten Zubeh rs oder Instruments an Varian oder einen Servicest tzpunkt erfolgen Der Kunde bernimmt die Verantwortung f r Verlust oder Besch digung im Transit und hat die Versandkosten im voraus zu bezahlen Var ian wird das Zubeh r oder Instrument vorausbezahlt und versichert zum Kunden zur ckschicken Anspr che f r Verlust oder Besch digung im Transit hat der Kunde zu erheben Zur Korrektur von Anomalien des Soft warebetriebs wird Varian Software Neuausgaben aus geben sofern Revisionen existieren und dies die beste Abhilfe ist Garantieeinschr nkungen Diese Garantie erfa amp t nicht vom Kunden bereitgestellte Software Ausr stungen und Software die von anderen Herstellern garantiert werden oder den Austausch ent behrlicher Teile und solcher von begrenzter Lebens dauer wie diese aber nicht darauf beschr nkt Filter Glaswaren Instrument Statuslampen Lampenquellen Septen S ulen Sicherungen Schreiberpapier und Tinte Zerst uber FluRzellen Kolben Dichtungen Fit tings Ventile Brenner Probenr hrchen Sondenein s tze Druckk pfe glasausgekleidetes Rohr Leitungs und Rohrfittings Dewars f r variable Temperaturen
119. the 216 LC instrument Setup Ethernet Ports for DH7XF1C1 10 190 76 121 x Address Module Type IP Address or Domain Name Status Actual IP a fa ic formen Online 10 190 76 146 _ 4 Ne No Address 46 None No Address 47 None No Address IP Address Management BOOTP Server No IP Addresses are being assigned from this Workstation etup Prompt for Setup if needed lt Back Cancel Figure 21 3 In the MS Workstation Configuration Menu ensure the 216 LC is moved from Available Modules to the Auto Start Box T System Control Configuration File Instrument Windows Help UOC No File Ele E Alte ro do O Instrument 1 MS Operator Vivian Roger Ready AutoStart Module E a 2 Instrument 1 Parameters Available 4000 QUAD Modules EE 1 42 30 216 LC Status and Control Window The following is the 216 LC Status and Control Window with the camera view on the right System Control NanoSpray System 1 Suspended mist MOR E File F Option O 22_full mth aer I oerte nl Capture C Window W Help H Instrun 216 LC 44 Ready r Run Status Pump Status Valve Status Runtime 0 00 min Reset Pump Flow Setpoint Actual Flow Pressure bar Available Volume uL amp Flow Endtime 25 00 min A 0 0 nL min 65 5 nL min 87 2 833 B Flow Q Ready B 0 0 nL min 158 7 nL min 92 0 1163 Load No Fault 5 0 0 nL min N 0 0 1
120. til et l abri de la chaleur des rayons directs du soleil du gel ou des sources d allumage Marquer les bouteilles de mani re n avoir aucun doute quant leur contenu N utiliser que des connexions et r gulateurs agr s 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 lev es que la plus haute pression de sortie du r gulateur 03 914603 82 11 Mesures de s curit en CPG Syst me d chappement Les d tecteurs CPG install s dans une pi ce bien ventil e ne n cessitent pas de conduits sp ciaux d chappement except lorsqu ils sont destin s analyser des substances chimiques dangereuses Lors de l installation de tels conduits m N utiliser que des conduits l preuve du feu m Installer un ventilateur la sortie du conduit m Placer les orifices d aspiration de mani re ce que les vibrations ou les mouvements d air n affectent pas le fonctionnement du d tecteur m V rifier p riodiquement l tat du conduit m S assurer que le laboratoire est correctement ventil D tecteurs source radioactive m Se conformer au manuel d utilisation de ECD Ni en particulier ses NOTES MISES EN GARDE ET AVERTISSEMENTS m Effectuer les tests de d contamination radioactive d crits dans le manuel d utilisation de ECD Ni m Se conformer aux proc dures et au calendrier des essais
121. ung den gleichen Wert haben f r den das In strument verdrahtet ist Gasdruckflaschen 2 of 4 Lagern und handhaben Sie komprimierte Gase vorsichtig und in strikter Einhaltung der Sicherheitsvorschriften Befestigen Sie die Gasflaschen an feststehenden Aufbauten oder an W nden Lagern und transportieren Sie Gasflaschen in aufrechter Stellung Druckregler zuvor abnehmen Lagern Sie Gasflaschen in gut durchl fteten R umen weit genug weg von Heizungen direktem Sonnenschein Frosttemperaturen und Entz ndungszonen Kennzeichnen Sie die Flaschen so eindeutig da kein Zweifel ber deren Inhalt bestehen kann Benutzen Sie nur gepr fte Druckminderer und Verbindungsst cke Benutzen Sie nur chromatographisch reines Verbindungsrohr Varian Part Number 03 918326 00 das wesentlich h heren Druck als den h chsten Ausgangsdruck des Druckminderers aush lt 03 914603 81 11 GC Sicherheitspraktiken Abgassystem F r GC Detektoren die in einem gut durchl fteten Raum installiert sind ist keine spezielle Abgasf hrung erforderlich auBer wenn die Detektoren zum Testen gef hrlicher Chemikalien benutzt werden Wenn Sie eine Abgasf hrung installieren m Benutzen Sie nur feuerfeste F hrungen m Installieren Sie ein Gebl se am Ausgang m Ordnen Sie die Ansaug ffnung so an da ihre Er sch tterungen oder Luftstr mungen nicht die De tektorfunktion beeintr chtigen m Pr fen Sie regelm ig die einwandfreie Arbeits weise d
122. unt of nonvolatile material but at some expense in signal intensity To adjust the position of the vaporizer relative to the capillary entrance loosen the four mounting screws on top of the spray chamber and slide the vaporizer assembly forward or backward Use the numbered scale on the right of the vaporizer assembly to assist in resetting the position Tighten all four screws snugly when you are finished to avoid heat damaging the vaporizer It must be firmly attached to the spray chamber for proper heat sinking Typical APCI Operating Parameters WARNING BURN HAZARD APCI Source may become hot during operation Take appropriate precautions e Drying Gas 12 psi 2 Liters min at 150 C e Nebulizing Gas 60 psi 71 5 liters min Nitrogen in positive mode Air in negative mode Automatically switches if air is connected e Auxiliary Gas 17 psi 2 liters min as hot as possible without decomposing sample maximum temperature setting is 550 C e Corona Current 5 10 uA e Housing Temperature 50 C Atmospheric Pressure Chemical lonization APCI Performance Evaluation Operating Conditions for Testing the APCI e Drying Gas 12 psi at 150 C e Nebulizing Gas 60 psi at 550 C e Auxiliary Gas 17 psi e Corona Needle Current 5 uA e Housing Temperature 50 C e Solvent 50 50 methanol water at 1 mL min e Multiplier Set to optimum value e Scan Method 0 25 sec scan Mass peak width 1 0 SIM width 0 7
123. ure that voltage sources and line voltage match the value for which the instrument is wired Compressed Gas Cylinders 2 of 4 Store and handle compressed gases carefully and in strict adherence to safety codes Secure cylinders to an immovable structure or wall Store and move cylinders in an upright vertical position Before transport remove regulators and install cylinder cap Store cylinders in a well ventilated area away from heat direct sunshine freezing temperatures and ignition sources Mark cylinders clearly so there is no doubt as to their contents Use only approved regulators and connections Use only connector tubing that is chromatographically clean Varian Part Number 03 918326 00 and has a pressure rating significantly greater than the highest outlet pressure from the regulator 03 914603 00 11 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 m Use only fireproof ducting m Install a blower at the duct outlet Locate duct intakes such that their vibration or air movement does not effect detector operation m Check periodically for proper operation of the duct m Ensure proper ventilation in lab area Radioactive Source Detectors m Read carefully and comply with all NOTES CAUTIONS and WARNINGS in the Ni ECD manual m Perform
124. uses en question sous r serve du choix de Varian de rembourser une part raisonnable du prix d achat de l instrument ou de l accessoire La r paation ou le remplacement sous garantie n tend pas la p riode de garantie originale La r paration ou le remplacement aux termes d un recours est laiss l enti re discr tion de Varian soit par l envoi d un technicien de maintenance sur le site du client soit en autorisant le client retourner l accessoire ou l instrument d fectueux Varian voire l envoyer un service de maintenance d sign 03 914412 82 2 Le client assumera la responsabilit de toute perte ou sinistre lors du transport et r glera l avance les frais de transport Varian renverra l accessoire ou l instrument au client en port pay et assur Toute r clamation r sultant d une perte ou d un sinistre intervenu lors du transport devra tre faite par le client Aux fins de correction des anomalies de fonctionnement du logiciel Varian diffusera des mises jour des logiciels le cas ch ant et si de l avis de Varian elles constituent la mesure corrective la plus appropri e en la mati re Limitation de garantie Cette garantie ne couvre pas le logiciel fourni par le Client les quipements ou logiciels garantis par un autre fabricant ni le remplacement des pi ces consommables ou pr sentant une dur e de vie limit e notamment filtres verres indicateurs d tat de l instrument lampes
125. w PEEK fingertight ferrule and nut 28 211542 00 over the end of the PEEK tubing While ensuring that the PEEK tube is bottomed out gently tighten the fitting PEEK Tubing and Needle Assembly 03 937544 03 Nebulizer Assembly Replacing the APCI Quartz Tube It is possible for the quartz vaporizer tube to look dirty and not affect performance Replace the quartz tube only if performance degrades Keep the components as clean as possible to avoid contaminating the interface Atmospheric Pressure Chemical lonization 13 14 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 WARNING The spray chamber may contain hazardous chemicals CHEMICAL HAZARD Use appropriate protection when handling Removing the Quartz Tube 1 Cool the APCI vaporizer NOTE To cool the vaporizer leave the spray icon on and set the vaporizer temperature to zero Leaving the gases on carries away residual heat Turn the gases and voltages off by clicking the spray icon blue LED on the front of the instrument must be off Disconnect the gas lines from the bulkhead fittings on the front of the instrument Disconnect liquid connection to injector or column not the fitting on top of the nebulizer Disconnect the large round 14 pin conne
126. with the instruction manual may cause harmful interference to radio communications Operation of this equipment in a residential area is likely to cause harmful interference in which case the user will be required to correct the interference at his own expense 3 of 4 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 include relays lamps temperature probes detector elements motors etc Sheet metal parts structural members or assemblies and castings printed circuit boards and functional modules are normally capable of being rebuilt to like new condition throughout their useful life and therefore will be supplied only on an as available 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 basis after the final production run of the instrum
127. 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 est Intentamos comprender las necesidades de nuestros clientes a trav s de entidades independientes grupos de usuarios oficinas de asesoramiento a usuarios y nuestro programa de respuesta Hallmark of Quality adem s de los contactos directos con nuestros clientes Nuestros productos y procedimientos est n dise ados para poder corresponder a sus necesidades Sabemos que nuestros clientes buscan m s 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 QUALITY SYSTEM 1010 9001 Nuestra meta principal es ser ese socio E 03 914451 84 4 1 of 1 Instrumentos analiticos Varian Inc Garantia Productos hardware Todos los instrumentos analiticos vendidos por Varian Inc est n garantizados contra defectos de materiales y de fabricaci n por la duraci n especificada y de acuerdo con los t rminos establecidos en las ofertas de Varian o seg n lo especificado en el acuerdo escrito entre Varian y el cliente El plazo de garant a comienza a partir de la fecha de env o del material de Varian al cliente original Sin embargo si la instalaci

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