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ProStar 355 Refractive Index Detector

1. nennen 95 Adjustments itecto pono m ettet a leale 99 Testing of Flow Cell Integrity iii 100 Checking the Drain Tube sus 100 Using the Span Adjustment Procedure ii 101 Replacement of Flow Cell Assembly ss 102 Lro bleshootlng 4 2 a ed pe e ave ae peres 102 Testing the ProStar 355 in Stand Alone Mode sse 103 Troubleshooting a HPLC System us 103 Troubleshooting Table ss 104 Appendix doner 107 Specifications eL 107 Performance Specifications 107 General Specifications sente 107 Physical Specitications 42 alcalina ao 108 Physical Constants of Select Solvents nenn 109 Mis ibility Chart irc Ee Ear tie aptas 110 Polarity Index P rna e me ere aee Ene IRR IER SRI iei 111 ii 85 102195 00 2 Safety information Operating Instructions This instruction manual is provided to help you establish operating conditions which will permit safe and efficient use of your equipment Special considerations and precautions are also 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 instru
2. NOTICE This document contains references to Varian Please note that Varian Inc is now part of Agilent Technologies For more information go to www agilent com chem Varian Inc 679 Springvale Rd Mulgrave Victoria 3170 vie Australia 5 Agilent Technologies ProStar 355 Refractive Index Detector Operation Manual Overvoltage category II Pollution degree 2 Safety class 1 EN61010 1 QUALITY SYSTEM INO9001 C E R T I F I E D Varian Inc 2005 Printed in Australia 8510219500 Rev 2 Varian Inc offices Varian has offices in most countries The major offices for chromatography are listed below Varian Australia Pty Ltd Manufacturing site 679 Springvale Road Mulgrave Victoria 3170 Australia Phone 61 3 9560 7133 Fax 61 3 9560 7950 Varian Inc Analytical Instruments 2700 Mitchell Dr Walnut Creek CA 94598 USA Phone 1 800 FOR HPLC International Phone 1 925 939 2400 Fax 1 925 945 2360 Varian B V Herculesweg 8 4338 PL Middelburg The Netherlands Phone 31 0118 67 1000 Fax 31 0118 62 3193 Internet The Varian Inc Internet home page can be found at www varianinc com Varian Australia Pty Ltd is the owner of copyright on this document and any associated software Under law the written permission of Varian Australia Pty Ltd must be obtained before either the documentation or the software is copied reproduced translated or converted to electron
3. ATTENZIONE ATTENZIONE Questo strumento amp 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 Questo strumento progettato per l analisi cromatografica di campioni opportunamente preparati Deve essere utilizzato usando gas e solventi adatti a questo scopo ed entro i limiti massimi di pressione flusso e temperatura riportati in questo manuale Se lo strumento non viene utilizzato secondo le modalit specificate dal costruttore le condizioni di sicurezza previste potranno non essere sufficienti E responsabilit del Cliente informare il Servizio Tecnico Varian prima di qualsiasi intervento di riparazione se lo strumento stato utilizzato per l analisi di campioni biologicamente pericolosi radioattivi o tossici ProStar 355 Refractive Index Detector 31 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 polarita riportate nel manuale di istruzioni che quelle stabilite dalle norme di sicurezza del laboratorio Sostituire i fusibili bruciati solo con fusibili che
4. anthra napth Figure 15 Chromatogram of RI Test Mixture ProStar 355 Refractive Index Detector 89 Shutdown Procedures Corrosive Solvents Some solvents may corrode the detector if they are left in the detector and should be thoroughly flushed from the entire system including the reference and sample flow cell See Table 1 Solvent Limitation Recommendations The quartz cell window in particular is easily etched by strong bases Do not turn power to the ProStar 355 off without rinsing these solvents from the detector Some solvents can be left in the cells at the end of an operation For example water acetonitrile 2 propanol the xylenes and paraffinic hydrocarbons are quite innocuous They may be left in the ProStar 355 overnight or over a weekend No Flow Versus Reduced Flow 90 A continuous slow flow through the ProStar 355 is the preferable shutdown procedure especially if buffers tetrahydrofuran and organohalocarbons are in use Reduced flow may be 0 5 mL min to 0 01 mL min but the HPLC pump must be able to stay primed at reduced flow If the ProStar 355 is under external control you may alternate between Purge on and Purge off while you flush at reduced flow Buffers Even if the buffer is non corrosive see Solvent Recommendations page 63 and Corrosive Solvents page 90 it is better to keep the solvent flowing at a reduced rate to eliminate the possibility of salt precipitation in the ProStar 355 cells and
5. BREATHING HAZARD If you do install ducting Use only fireproof ducting Install a blower at the duct outlet Locate duct intakes such that their vibration or air movement does not affect detector operation Check periodically for proper operation of the duct Ensure proper ventilation in lab area 85 102195 00 2 SAFETY INFORMATION Radioactive Source Detectors WARNING RADIATION SOURCE m Read carefully and comply with all NOTES CAUTIONS and WARNINGS in the Ni63 ECD manual m Perform the tests for removable radioactive contamination described in the Ni63 ECD manual m Comply with leak test schedules and procedures Burn Hazard WARNING 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 ProStar 355 Refractive Index Detector 7 LC Safety Practices High Pressure Hazard If a line ruptures a relief device opens or a valve NS WARMING opens accidentally under pressure potentially hazardous high liquid pressures can be generated by the pump causing a high velocity stream of volatile 2 WARNING and or toxic liquids DD EXPLOSION HAZARD m Wear face protection when you inject samples or perform routine maintenance
6. 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 44 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 A AS VARIAN www varianinc com 85 102195 00 2 Introduction General Description x incident beam pl The ProStar 355 differential refractometer is a high performance universal detector designed for analyses requiring the continuous monitoring of the refractive index of a flowing liquid with respect to a reference Its small cell volumes high sensitivity excellent temperature control and flexible control options make it well suited for use as a detector in auto
7. 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 18 85 102195 00 2 INSTRUCCIONES DE SEGURIDAD Radiaci n Ultravioleta Los detectores del Cromat grafo de Liquidos 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 situada durante su funcionamiento m No mire directamente a las celdas del detector a la fuente de luz UV Cuando inspeccione la fuente
8. Operation How to Use This Section This section provides guidelines for the operation of the ProStar 355 The following topics are covered e Solvent limitations recommendations and preparation e Sample preparation e ProStar 355 controls e Pre operation check list e Instrument operation e Initial test procedures e Examples of use e Shutdown NOTE To document the performance of your new ProStar 355 detector for future reference perform the following tests and archive the results 1 Noise and Drift Test see page 81 2 Chromatogram of RI Test Sample see page 88 and Figure 15 Solvent Recommendations Solvent Limitations Some solvents may corrode the wetted surfaces of the ProStar 355 detector if they are left in the detector after operation The quartz cell window is easily etched by strong bases It is recommended that some Solvents be rinsed from the ProStar 355 detector for overnight and ProStar 355 Refractive Index Detector 63 weekend storage Refer to Table 1 Solvent Limitation Recommendations The solvents used in the ProStar 355 detector are limited by the materials used for the hydraulic parts they come in contact with e g quartz glass PTFE and 316 stainless steel These limitations should be considered in selecting mobile phase solvents NOTE Table 1 is intended to serve as a guide and does not cover all possible conditions Since actual effects depend upon a number of conditions te
9. ProStar 355 detector Verify that the detector is stable before continuing Perform steps 6 and 7 of the recorder procedure beginning on page 77 Note that you have been instructed to flush the reference cell with sucrose solution If the cells are intact the recorder pen will deflect 50 5 Integrator H output will measure approximately 820 mV 50 mV However if the cells are broken the measured deflection will be noticeably diminished This is because the water of the reference cell and the sucrose of the sample cell will dilute each other making the span apparently out of adjustment at each successive attempt Do not conclude that the flow cells are ruptured prematurely Retest the flow cells if a rupture is indicated 101 Replacement of Flow Cell Assembly To replace a flow cell assembly contact your Varian Customer Support Representative This is not a recommende procedure for the user Troubleshooting Malfunctions within the ProStar 355 can arise from three general sources e The ProStar 355 itself can be dirty or operating non optimally e The HPLC system can have a broken dirty or non optimally operating component but the problem is manifesting itself in the ProStar 355 detector e A mobile phase and or column problem which by its very nature is spread throughout the HPLC system but appears as a malfunction of the ProStar 355 detector To troubleshoot the ProStar 355 you must be able to separa
10. 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 A AS VARIAN www varianinc com 85 102195 00 2 SICHERHEITSINFORMATIONEN Sicherheitsinformationen Arbeitsanleitungen Diese Arbeitsanleitung will Ihnen bei der Aufstellung solcher Arbeitsbedingungen helfen die einen sicheren und wirkungsvollen Gebrauch Ihrer Ger te erm glichen Besondere berlegungen und Vorsichtsma nahmen erscheinen in diesem Handbuch in Form von HINWEIS ACHTUNG und WARNUNG wie unten beschrieben Es ist wichtig da 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 ACHTUNG Weist auf Situationen die zu m iger Beeintr chtigung und oder zu Ger tesch den f hren und auf die Vermeidung dieser Situationen hin WARNUNG Weist auf m gliche Gefahrensituationen die zu ernsthaften Verletzungen f hren k nnen und auf die Vermeidung dieser Situationen hin ProStar 355 Refractive Ind
11. 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 ProStar 355 Refractive Index Detector 25 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 a 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 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 certains solvants sont susceptibles de provoquer des faiblesses et des fuites avec risques d explosion Tous les cons
12. types of power socket Use only the power cable provided WARNING FIRE HAZARD Do not use the detector in places where combustible gas or any source of fire or sparks might exist Loosening the Shipping Bolts The Varian ProStar 355 is shipped with the optical module securely tightened down by two Allen bolts These bolts must be loosened so the optical system can rest on rubber shocks that will isolate the optics from vibration 1 Refer to Figure 3 Gently place the right side of the detector on the end of a bench while supporting it to prevent it from falling ProStar 355 Refractive Index Detector 53 e ae Bottom View Figure 3 Loosening the Shipping Bolts 2 Locate the 6 bolts in the ProStar 355 floor panel Loosen the two center bolts one full turn counterclockwise using the 5 mm Allen key in the Accessory Kit NOTE Do not loosen all 6 bolts Do not remove the bolts Do not run them out so far that the detector s weight rests on the bolt heads instead of its feet 3 Move the detector securely back onto the bench NOTE Detector will not stabilize if shipping bolts are not loosened Optics Module Drain Tube The drain tube attachment for the optic module allows liquid to drain from the module if a sample or reference cell should break The tube exits the side of the instrument Connect PTFE tubing 6 mm OD 4 mm ID to this port Lead the tubing to a safe waste disposal
13. 120 Vac 60 Hz applications is terminated in a 3 prong parallel blade plug requiring a matching receptacle wired as shown in Figure 2 Outside of the 120V 60 Hz area the instrument is supplied with a power cord terminated in a Schuko CEE 7 7 2 prong plug Replacement of the instrument power plug 50 85 102195 00 2 INSTALLATION requires strict compliance with power cord color coding as listed in Figure 2 NOTE Potentialbetween neutraland ground should not exceed 3 volts Neutral 5 A Hot Line Ground 15Amps 220 Vac Nominal 120 Vac Nominal 50 Hz 60 Hz CAUTION This instrumentis designed for single phase operation ONLY Ground green yellow or green Neutral It blue or white Hot brown or black Figure 2 Power Cord Wiring Power Button Fuse amp Grounding The ProStar 355 Power button is located on the bottom left of the front panel The power should OFF before connecting the power cord to the detector The receptacle for the power cable is located on the rear of the detector A 3 15 A fuse is provided The fuse will be installed as described on page 52 in Installing the fuse and power cable Ground the detector using the grounding cable supplied in the Accessory Kit Connect the circular end to one of the grounds on the back panel see Figure 5 and the alligator clip end to a known ground ProStar 355 Refractive Index Detector 51 WARNING SHOCK HAZARD Electrically conducting sp
14. Chromatography has a tendency to cause baseline drift due to oxidation during analysis and therefore requires the addition of an anti oxidant However the addition of an anti oxidant may cause the eluent to be unusable with a UV detector due to absorption by the anti oxidant All solvents including deionized water should be filtered with a 0 45 um or 0 2 um filter Filtering protects the pump injector and column from potential damage and early failures due to large particles adhering to surfaces Vacuum filtration functions to filter and degas solvents ProStar 355 Refractive Index Detector 65 Solvent Degassing All solvents must be properly degassed prior to use on the ProStar 355 detector Solvents that are not properly degassed may cause bubble formation in pump heads and in the detector cells potentially causing pressure flow problems and a noisy chromatographic baseline Degassing is especially important when the column temperature is elevated above room temperature or with solvents that have a high gas solubility e g methanol Analysis times that run greater than 5 to 6 hours will also require degassing of solvents Solvents can be degassed by vacuum degassing filtration stirring ultrasonic agitation sparging with helium or an in line degasser may be used Vacuum filtration of solvents through a 0 2 uum or 0 45 um membrane filter is a convenient method to both degas and filter solvents Varian Aqueous and Organic Solvent
15. Informations ei si nano 1 Introd HC HOD nn Nr iia 45 General Description citar 45 AA ELLE UC cana 47 Unpacking and Inspection sis 47 Do s and Don ts of RI Detectors eene nennen nnne nnns 48 Installation Site Requirements eene nennen nns 48 Power REQUIEM iaa alien 50 Power Button Fuse amp Grounding nennen 51 Preparing the ProStar 355 for Operation 52 Installing the fuse and power cable en 52 Loosening the Shipping Bolts nennen 53 Optics Module Drain Tube 54 Tubing Connections to the ProStar 355 55 Connection to the Inlet ccrte irte rite een 55 Connection on the Outlet Side 56 Cable Connections to the ProStar 355 sss eene 56 Recorder Connection issue 56 Integrator Connection is 56 Connection to a Varian Star 800 Module Interface Box sss 58 Connection to a Varian Star Chromatography Workstation en 59 Connection to a Varian 4400 Integrator 59 External Control of the ProStar Ia beste ue ee ct tes 60 A E ET TET I 63 H w t Us This Section iti t i fr realen ea 63 Solvent Recommendations ss 63 Solvent Limitations onere eat 63 General Recommendations for Solvent Preparation 65 Sample Preparations e lac sani RUD ioni 66 ProStar 355 Controls ia edP ate ede bin cree Pip eisen 67 Bl
16. OUT sensitivity 2 mV uRIU or 8 mV uRIU integrator range 500 uRIU V or 125 uRIU V 85 102195 00 2 N WARNING DANGEROUS VOLTAGES SED WHEN COVER IS REMOVED UNPLUG POWER CORD ZN WARNING FOR CONTINUED PROTECTION REPLACE ONLY WITH SAME FUSE TYPE AND RATING CE This Equipment complies with the requirements in Part 15 of FCC Rules for a Class computing device Operation of this equipment in a residential area may cause unacceptable interference to radio and TV reception requiring the operator to take whatever steps are necessary to correct the interference INSTALLATION N N t SEE MANUAL A 250V LINE 100 240V POWER MAX FREQUENCY T3 15A Figure 5 Rear Panel Controls Purge terminals PURGE IN When these two terminals are short circuited the flow line of the eluent is changed and both sample and reference cells are filled with the same eluent as occurs when the Purge key is pressed Zero in terminals ZERO IN When these two terminals are short circuited an Auto Zero is activated as occurs when the Zero key is pressed Marker in terminals MARKER IN When these two terminals are short circuited a momentary voltage spike is put on top of the recorder output as occurs when the Marker key is pressed Ready out terminals READY OUT A contact pulse is sent out through these terminals when the sequence is completed Leak out terminals LE
17. This is the static drift See Figure 13 for an example If drift is outside of specifications check to see if there are noticeable temperature fluctuations in the lab environment If so repeat the drift test with the ProStar 355 in an enclosure such as a cabinet or box 83 84 1 Collect at least 30 minutes 9 5x10 RIU of baseline at range of 1 x 10 RIU FS 2 Draw two parallel lines such that all data are enclosed yet the distance between the lines is minimized 3 Find the slope of either line in RIU Hr so a BC 0 5hr b AB 9x10 RIU SLOPE 9x10 RIU 0 5hr 18x10 RIU hr Noise 1 8 x 10 RIU hr Figure 13 Example Drift Test Data of the ProStar 355 Detector 85 102195 00 2 NOISE 10 11 12 13 ProStar 355 Refractive Index Detector OPERATION Set attenuation REC RANGE Y If instrument is not fully equilibrated the signal will be very erratic You may choose to monitor on REC RANGE 1 until the signal is stable then monitor at REC RANGE until signal is stable at that setting then finally monitor at REC RANGE Y Collect 20 minutes of signal The pen cannot go off scale during any portion of this 20 minute period Divide the 20 minutes of signal trace into 1 minute segments with vertical lines For each minute segment draw two parallel lines so that the entire minute of si
18. con fuentes radioctivas m Leacon cuidado y cumpla todas las NOTAS PRECAUCION y ATENCION del Manual del Detector Ni63 ECD m Realice los test de contaminaci n radioactiva descritos en el Manual del Detector Ni63 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 6 fr as durante bastante tiempo despu s de apagar el instrumento Para evitar quemaduras asegureses de que todas las reas que se calienten enfr en han vuelto a la temperatura ambiente protejase adecuadamente las manos antes de tocar las superficies potencialmente calientes 6 fr as ProStar 355 Refractive Index Detector 17 LC Pr cticas de Seguridad Peligro de Alta Presi n Si se rompe una linea de presi n 6 se abre una v lvula de seguridad accidentalmente bajo presi n la bomba puede generar liquidos a alta presi n potencialmente peligrosos produciendo un chorro a alta velocidad de liquidos volatiles y 6 t xicos m Lleve protecci n facial cuando inyecte muestras 6 realice mantenimiento de rutina 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 que 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
19. container 54 85 102195 00 2 INSTALLATION WARNING SHOCK HAZARD Electrically conducting spills can occur when conductive HPLC solvents are spilled on or in the instrument Ground the instrument properly to protect the operator from electrical shock Proper grounding also protects the instrument from power line noise Verify that the instrument is properly grounded through the power line ground terminal Do not remove or otherwise disable the power cord ground prong Tubing Connections to the ProStar 355 To maximize performance of the ProStar 355 and minimize back pressure to the refractive index cells review Do s and Don s of RI Detectors Connection to the Inlet NOTE The ProStar 355 must be the last component in any LC system No detector or backpressure regulator can follow it Do not use narrow bore tubing after the ProStar 355 Refer to Figure 4 1 Install the narrow bore stainless steel tubing from the Accessory Kit 0 25 mm ID 1 m long and Parker Hannifin nut and ferrule into the IN fitting of the ProStar 355 Swage the ferrule securely onto the tubing with the nut 2 Connect the opposite end of the tubing in the same manner to the column exit end See Figure 4 Pumping ax System DO 3 Column Detector H IN Injector OUT Waste ProStar 355 Figure 4 ProStar 355 connected to the HPLC System ProStar 355 Refractive Index Detector 55 Connection on the Ou
20. de luz 6 la celda utilice siempre una protecci n para los ojos como gafas de borosilicato 6 poliestireno 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 afios 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 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 ultimo instrumento fabricado Disponibilidad de Servicio Varian ofrece una gran variedad de sistemas de Servicio para mantener el soporte a sus usuarios tras el periodo de garant a 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 ProStar 355 Refractive Index Detector 19 Oficinas de Instrumentaci n Analitica Varian Pa
21. equilibrate with a syringe e Fillthe 5 mL syringe with deionized water e Connect the syringe needle to the IN port of the ProStar 355 e Press Purge flow path will include both sample and reference cells e Inject 4 5 mL of water into the IN port NOTE It is normal to feel considerable backpressure on the syringe A 1 3 mL syringe e g Varian part number 0099672118 2 5 mL can be used in place of the 5 mL syringe for less pressure 5 Select a range of 512 x 10 RIU 6 After the detector signal output stabilizes Auto Zero to adjust optics and signal and signal zero to recorder zero For further details see paragraph 3 6 1 Monitor signal to verify that everything is zeroed and stable 7 With Purge off using the 5 mL syringe inject 2 3 mL of the standard sucrose solution prepared in step 1 into the IN port and allow to equilibrate several minutes This fills the sample cell with the standard solution 256 x 10 RIU is now obtained referenced to the deionized water in the reference cell 8 The recorder pen should have deflected by 50 10 of full scale If it does not and you are certain the recorder is correctly set and calibrated adjust the span by turning the VR2201 potentiometer on the Amplifier Board with a small ProStar 355 Refractive Index Detector 79 80 screwdriver until the recorder registers 50 of full scale Refer to Figure 3 6 for an example of span test recorder output 9 Integrator
22. 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 einschlie lich Leitungen und Sammelgef e 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 42 85 102195 00 2 SICHERHEITSINFORMATIONEN Ultraviolette Strahlung Detektoren in Liquidchromatographen die eine ultraviolette Lichtquelle benutzen besitzen eine Abschirmung die das Bedienungspersonal gegen Abstrahlungen sch tzt Zum st ndigen Schutz m Achten Sie darauf da die sch tzende Lampenabdeckung 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 Inspizieren der Lichtquelle oder der Fl ssigkeitszelle benutzen Sie immer einen wirksamen Augenschuiz wie er durch Borsilikatglas oder Polystyrol gew hrleistet wird Verf gbarkeit von Ersatzteilen Es ist Varian s Grundsatz Ersatzteile f r alle Instrumente und die wichtigsten Zubeh re f r einen Zeitraum von f nf 5 Jahren nach dem Fertigungsauslauf dieser Ger teserie verf gbar zu haben Nach diesem Zeitra
23. hei e oder kalte Oberfl chen ber hren ProStar 355 Refractive Index Detector 41 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 gef 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 m ffnen Sie niemals eine unter Druck stehende L sungsmittelleitung oder ein Ventil Halten Sie zuerst 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
24. optics module and clean it with methanol and a lint free wipe Reassemble lamp and socket in the optics module Tighten the locking ring by hand then tighten the locking ring setscrew with a 1 5 mm Allen wrench 4 Turn power on Check alignment of the filament and the light pattern on the slit Repeat steps 2 and 3 if necessary 5 Replace inside cover polyurethane foam insulate outside cover and case cover 6 Check span adjustment per page 77 Testing of Flow Cell Integrity Replacement of the ProStar 355 flow cells is a non routine exacting procedure Only Varian Customer Support Representatives should replace flow cells Additionally the cells are well hidden from inspection Therefore the following procedure is offered for determining if the cells have ruptured without disassembly of the ProStar 355 The flow cell can be purchased only as part of the flow cell assembly Checking the Drain Tube The simplest way to check for cell rupture is to observe liquid coming out of the drain tube on the rear panel when liquid is flowing through the detector However the optics module would have quite a bit of liquid in it before liquid appears in the drain tube 100 85 102195 00 2 MAINTENANCE AND TROUBLESHOOTING Using the Span Adjustment Procedure 1 ProStar 355 Refractive Index Detector Follow Recorder and Integrator Span Test and Adjustment on page 77 After flushing the sample cell well with water re zero the
25. out nor fatigued filament is found double check for other possible problems in your ProStar 355 see Troubleshooting page 102 Any adjustment of the lamp will necessitate lamp alignment and span adjustment 97 3 To replace the lamp assembly remove the Pre amplifier PC Board and remove the lamp power cable from its connection on the barrier strip on the inside of the front panel Loosen the locking ring setscrew 8 in figure below with a 1 5 mm Allen wrench Turn the lamp socket locking ring counterclockwise and remove the lamp assembly 4 Hold the new lamp socket assembly as indicated in Figure 18 Notice that the lamp filament 1 is aligned with the vertical axis as is one of the three setscrews 8 as shown in Figure 19 It is important that the filament not the lamp s bulb be centered within the concentric circles of the lamp Socket Leave the locking ring setscrew and lamp socket locking ring slightly loose for the light pass adjustment page 99 Connect the spade lugs of the lamp power cable to its terminals 5 Proceed immediately to page 99 Adjustments Lamp Socket Locking Ring Socket Holder Socket Setscrew 1 of 3 Lamp Power Cable Spade Lugs 2 Locking Ring Setscrew 1 o bo OT oq L Items 1 4 and 6 constitute the Lamp Assembly 0392602810 on the ProStar 355 Figure 18 Lamp Assembly Exploded View 98 85 102195 00 2 MAINTENANCE AND
26. service d assistance a la client le ou pour passer commande de pieces 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 28 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 A VARIAN www varianinc com 85 102195 00 2 INFORMAZIONI SULLA SICUREZZA Informazioni sulla Sicurezza Instruzioni per l Uso Questo manuale ha lo scopo di aiutare l op
27. span adjustment tracks with the recorder span Therefore to set integrator span repeat steps 4 through 7 ignore step 5 as range setting is not relevant to an integrator With a volt ohmmeter measure the voltage at the integrator output positive H and negative 0 terminals The volt ohmmeter should show a response to the sucrose solution of 820 mV 50 mV H 0 in reference and sample cells AC Sucrose solution injection begins From syringe handling 2 mL sucrose solution _ completely injected P H O flush begins AC lt lt 2 mL H O flush finished A Conditions Range ProStar 355 512 x 10 FIU FS 35 C Figure 12 Recorder Span Adjustment 10 Carefully flush the sample cell with water The pen should return to its original zero point setting 11 Repeat steps 5 through 8 to confirm reproducibility 12 Reassemble the ProStar 355 85 102195 00 2 OPERATION Noise and Drift Test Noise and drift are measured according to ASTM Method No E 1303 95 for Refractive Index Detectors used in Liquid Chromatography For comprehensive information refer to that ASTM method The ASTM method also covers Flow Sensitivity Minimum Detectability Linear Range Dynamic Range and Calibration Specifications for the Varian ProStar 355 follow Noise 2 5 x 10 RIU static H O in cell temperature at 35 C for 2 hours Drift 2 5 x 107 RIU hr under same conditions Measure drift before noise because noise requires th
28. 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 85 102195 00 2 INFORMAZIONI SULLA SICUREZZA Norme di Sicurezza Per lavorare in modo sicuro sullo strumento Vi consigliamo si adottare le seguenti procedure m Verificare periodicamente che non ci siano perdite sulle linee e sui raccordi pneumatici m 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 m solventi organici vanno conservati in armadi speciali antiincendio ventilati e con indicazioni chiare sul contenuto di materiali tossici e o infiammabili m Non accumulare i solventi utilizzati Adottare un programma regolare di smaltimento ma mai nelle acque di scarico AVVERTENZA
29. AK OUT A contact pulse is sent out through these terminals if there is an eluent leak Error out terminals ERROR OUT A contact pulse is sent out through these terminals when an error occurs such as overheating null glass home position optical balance error lost parameters and low light intensity Integrator terminals INTEG OUT Signals to the data processing unit are sent out through these terminals The sensitivity of the output signals is 2 mV uRIU or ProStar 355 Refractive Index Detector 57 8 mV uRIU integrator range 500 uRIU V or 125 uRIU V Ground terminal for cable shield FG The shield of the provided signal cable should be connected to this terminal Recorder terminals REC OUT Signals to the recorder are sent out through these terminals The sensitivity of the output signals is 10 mV FS Communication port COM RS232C Communication port Ground terminals Terminals to ground the main body of the detector Power connector The power cable provided should be plugged into this connector Connection to a Varian Star 800 Module Interface Box The Star 800 Module Interface Box MIB provides analog to digital signal conversion ADC Connections are made by connecting a round miniDIN connector to one of the analog signal input ports on the middle right side of the Star 800 MIB For more information about connecting your ProStar 355 to a Star 800 MIB refer to your S
30. AUTION Do not use a backpressure regulator on the waste outlet side of the ProStar 355 6 Leave the system powered continuously for daily operation Before using the high sensitivity range it is best to leave the system temperature control on overnight Power Requirements The ProStar 355 detector requires a clean 50 or 60 Hz single phase power source capable of providing up to 0 8 amps at 100 120 Vac or 0 4 amps at 200 240 Vac NOTE Running the ProStar 355 detector on a voltage other than the correct single phase supply will void the warranty A separate circuit free of equipment with intermittent start and stop cycles and or heavy starting current demands is recommended for each instrument A measured GROUND to NEUTRAL potential of greater than 3 volts AC or DC indicates grounding problems that may need correction before connecting an instrument to the power source Any power source suspected of having noise problems should be evaluated with a recording power line monitor prior to being used for operating instruments NOTE Varian instruments are designed for use on single phase phase neutral power ONLY If your facility provides only phase phase i e three phase power consult the nearest Varian facility for information about isolation transformers BEFORE applying power to your instruments For phone numbers of Sales and Service Assistance refer to the Safety section The power cord for use in the US and other
31. Clarification Kit part number 0099750700 is available for this purpose Sample Preparation Generally it is desirable to dissolve samples in the mobile phase solvent When a different solvent is used a large solvent peak may appear on the chromatogram All particulates larger than 0 5 u must be removed Sample filtration kits are available for this purpose and can be found in the Varian Inc Consumables and Supplies catalog If filtration is inconvenient a pre column filter or guard column should be installed 66 85 102195 00 2 OPERATION ProStar 355 Controls Block Diagram and Basic Circuitry of the ProStar 355 Figure 8 is a block diagram of the ProStar 355 Refractive Index Detector Figure 9 shows the basic circuitry of the ProStar 355 input and output signals Optics Module Heat Exchange Block O Integrator Out D Recorder Out 1 Light source 9 Amplifier 2 Flow cell 10 Autozero circuit 3 Mirror 11 Sensitivity selection 4 Rough adjustment lens 12 Polarity selection recorder 5 Optical balance lens 13 Polarity selection integrator 6 Photodiode 14 Fine zero adjust 7 Solenoid Valve 15 Marker signal 8 Initial circuit 16 Power supply Figure 8 ProStar 355 Refractive Index Detector Block Diagram ProStar 355 Refractive Index Detector 67 This pulse must Digital Ground be more than 600 msec T Rated capacity of i Output Marker 500 mA 30 Vdc 1 pulse 0 5 sec Figure 9 Input Output Termi
32. 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 m Ozone can be generated by radiation from the source lamps Exposure to ozone can result in severe irritation to the skin eyes and upper respiratory system The maximum permissible exposure level is 0 1 ppm 0 2 mg m for 8 hours per day ALWAYS ventilate the area surrounding the detector such that the concentration of ozone does not exceed the maximum permissible level All venting must be to outside air never within the building ProStar 355 Refractive Index Detector 9 CE compliant products Your ProStar 335 Photodiode Array Detector has been designed to comply with the requirements of the Electro magnetic Compatibility EMC Directive and the Low Voltage electrical safety Directive commonly referred to as the LVD of the European Union Varian has confirmed that the product complies with the relevant Directives by testing a prototype against the prescribed EN European Norm IEC or CISPR standards Proof that the product complies with the Directives is indicated by m The CE marking appearing on the rear of the product m The documentation package that accompanies the product containing a copy of the Declaration of Conformity This Declaration is the legal declaration by Varian that the product complies with the Directives and al
33. If the span is outside this range NG will be displayed Recorder and Integrator Span Test and Adjustment Span adjustment for chart recorder and integrator may shift after any of the following procedures have been performed 1 Source lamp replacement 2 Photodiode replacement 3 Cell replacement Use the following procedure for recorder and integrator span testing and adjustment These are the items you need to perform this test e ProStar 355 with signal cable from REC OUT to a recorder set at appropriate voltage 1 mV or 10 mV e 5 mL glass syringe with Luer tip from Accessory Kit e 16 Luer needle with nut and ferrule from Accessory Kit e Smallflat bladed screwdriver from Accessory Kit e Small Phillips screwdriver from Accessory Kit e Approximately 600 mL H20 deionized degassed e Sucrose e Analytical balance accurate to 1 mg e 500 mL volumetric flask e An accurate volt ohmmeter for integrator span adjustment ProStar 355 Refractive Index Detector 77 78 Location of Daughter Boards Remove the cover of the ProStar 355 with the Phillips screwdriver Locate the VR2201 Blue trimming potentiometer with the Red mark on the Amplifier PC Board located in Daughter PC Board area see figure below Turn ProStar 355 power on Set the temperature to 35 C Front Barrier Strip er OO Spade lug connectors p from lamp and valve Solenoi
34. TROUBLESHOOTING Light Bulb Socket ight Bulb Socke Vertical Axis Filament Horizontal Axis Setscrew Longitudinal Axis of Bulb Socket Figure 19 Orientation of Filament in Lamp Socket Adjustments Two adjustments are necessary with lamp replacement optical alignment of the lamp and span adjustment Span adjustment is covered on page 77 1 Optical adjustment of lamp Remove the optics module cover Figure 17 Remove the polyurethane heat insulator and remove the inside cover beneath it If power is not yet on turn it on at this time 2 The figure below shows how the light from the source lamp should engulf and be centered around the slit entrance Adjust the light pattern using the three lamp setscrews Keep the filament aligned with the vertical axis You may need to press the lamp assembly slightly in and out if the light pattern is slightly off centered Sometimes it is more appropriate to press the lamp assembly in the direction opposite the offset When the light is centered tighten the locking ring while holding the lamp assembly firmly in position When optimal adjustment is attained tighten the setscrews ProStar 355 Refractive Index Detector 99 _ Light Pattern Slit Vertical Axis Horizontal Axis LI Pos Window Axis from ProStar 350 352 Front to Back Figure 20 Optimal Light Pattern on Flow Cell Slit 3 Turn power off Remove the lamp and socket from the
35. TY INFORMATION 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 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 ProStar 355 Refractive Index Detector 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 11 12 85 102195 00 2 INSTRUCCIONES DE SEGURIDAD Instrucciones de Seguridad I
36. abbiano le stesse caratteristiche queste ultime sono riportate sul pannello dei fusibili e o nel manuale di istruzioni Sostituire immediatamente i cavi di alimentazione difettosi o consumati con cavi dello stesso tipo e con le stesse caratteristiche Assicurarsi che il voltaggio del pannello di alimentazione corrisponda a quello dello strumento da collegare Bombole dei Gas 32 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 qualita Usare solo tubazioni cromatograficamente pulite Numero di Parte Varian 0391832600 e calibrate per pressioni superiori a quella massima di uscita dal manometro 85 102195 00 2 INFORMAZIONI SULLA SICUREZZA Procedure di Sicurezza in GC Scarico dei Gas Per i rivelatori GC non amp richiesto alcun sistema particolare di scarico dei gas se lo strumento amp installato in una stanza ben ventilata e se non viene utilizzato per l analisi di sostanze chimiche pericolos
37. allation site in accordance with the Do s and Don ts in the previous section Temperature fluctuation and airflow will affect the performance causing drift noise unstable baseline etc The following locations should be avoided 48 e Near an air conditioner e Near heating equipment especially cycling ovens e Areas exposed to direct sunlight e Near a ventilation fan e Near vibration sources e Near openable windows and doors 85 102195 00 2 INSTALLATION e Near sources of electrical noise e Areas where corrosive gases exist e Dusty areas Allow sufficient bench space for peripheral instrumentation and to satisfy the following additional installation site requirements 1 System pressure fluctuations will be measured as density variations by the ProStar 355 detector Use a high performance pumping system with no flow pulses to minimize the baseline noise level For Varian Star 9000 series pumps and Varian 5000 5500 pumps or ProStar 210 215 pumps make sure the pump is operating at 100 atm of backpressure and that the pulse damper is functioning properly The backpressure can be achieved either by the column itself or a coil of O 005 ID tubing placed between the pump and the column If pulse damping is needed use the Varian Pulse Reduction Accessory part number 0391970101 or the Ultra High Pulse Reduction Accessory part number 0391970102 For the PrepStar SD1 pumps no special operating pressure is required 2 The entir
38. cessoires 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 clientele 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 ProStar 355 Refractive Index Detector 27 Points de vente des instruments analytiques Varian Contactez votre point de vente r amp gional Varian pour toute question commerciale ou de
39. chloromethane ethyl ether and many fluorocarbons Recorder or signal cable from the detector to the recorder is faulty or shorting Electrical transients from power line or radio frequency source 104 Solution Purge pump heads Use only premixed degassed mobile phase Elevate waste reservoir above the level of the detector cells to create slight backpressure Note Do not add restrictor to waste line Premix and degas mobile phase Clean flow cells Refer to Cell Cleaning procedure on page 93 Test lamp and replace or adjust as necessary Refer to Lamp Test procedure on page 95 Move detector to a more stable environment Place cover over the detector Reduce or turn temperature off Cool mobile phase column and detector Modify method to exclude or decrease concentration of troublesome solvent Repair or replace detective cable Examine all connections Isolate the detector power source from other heavy equipment motors etc Use an EMI RF power line filter to remove voltage spikes Ground the detector to earth 85 102195 00 2 Problem Cause Noise appearing after 8 10 hours of operation Formation of gases in the mobile phase reservoir Noise cyclical Environmental temperature fluctuation Bubbles in reference cell Noise Waste line too small cyclical matching pump stroke frequency Damper has inadequate damping capacity for system Damper is operating at a pres
40. d Valve 00 997559 31 Lamp Assembly underneath Pre amplifier Board 03 926028 10 Pre amplifier Board 03 926028 02 Optics Module Figure 11 Interior Components of the ProStar 355 2 Preparation of standard sucrose solution Weigh out 853 mg sucrose and transfer quantitatively to a 500 mL volumetric flask Dissolve in the deionized filtered degassed water and dilute to flask mark The refractive index of this standard solution is 256 x 10 RIU referenced to deionized water at room temperature NOTE Use the sucrose solution within one week Keep refrigerated 3 Prepare the syringe and needle by placing the nut and ferrule onto the end of the needle inserting the needle into the IN port of the ProStar 355 until it bottoms out Hold the needle with one hand and swage the ferrule onto the needle with the 5 16 wrench Remove the needle and assemble it to the syringe Equilibrate the ProStar 355 by pumping deionized water through both the reference and sample cells or with the 85 102195 00 2 OPERATION syringe inject deionized water into the two cells Use the same deionized water as that used to prepare the sucrose standard solution To equilibrate with a pump e Set pump flow rate to 1 mL min e Let flow for 5 minutes e Press Purge flow path will include both sample and reference cells e Let flow for 5 minutes e Press Purge flow path excludes reference cell To
41. d back strain or injury by following all precautions for lifting heavy objects WARNING BREATHING HAZARD Hazardous fumes may be present Do not inhale fumes Wear a face mask if required This symbol may be used on warning labels attached to the instrument When you see this symbol you must refer to the relevant operation or service manual for the correct procedure referred to by that warning label 85 102195 00 2 SAFETY INFORMATION Information symbols The following symbols appear on the ProStar 335 detector to provide you with additional information I Mains power on O Mains power off Single phase alternating current ES Fuse Appears on the rear of the product to indicate that the product complies with the C requirements of one or more EU Directives General Safety Precautions Follow these safety practices to ensure safe equipment operation m Perform periodic leak checks on all supply lines and pneumatic plumbing m Do not allow gas lines to become kinked or punctured Place lines away from foot traffic and extreme heat or cold m Store organic solvents in fireproof vented and clearly labeled cabinets so they are easily identified as toxic and or flammable materials m Do not accumulate waste solvents Dispose of such materials through a regulated disposal program and not through municipal sewage lines ProStar 355 Refractive Index Detector 3 Federal Communications Commission advi
42. e Se si deve installare un sistema di scarico dei gas m Usare condutture non 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 Ni63 m Eseguire tutti i test di contaminazione radioattiva rimovibile descritti nel manuale dell ECD al Ni63 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 ProStar 355 Refractive Index Detector 33 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
43. e ProStar 355 to be operating at maximum sensitivity To perform both tests you need the following equipment e ProStar 355 with signal cable from REC OUT to a recorder set at appropriate voltage 1 mV or 10 mV or from INTEG OUT to an integrator e 5mL glass syringe with Luer tip and 16 needle with ferrule and nut from Accessory Kit e Degassed filtered deionized water about 50 mL 1 Turn ProStar 355 power and temperature control ON Equilibrate unit at 35 C Room temperature must be greater than 18 C for the ProStar 355 to maintain 35 C internal temperature 2 Prepare the syringe and needle by placing the nut and ferrule onto the end of the needle inserting the needle into the IN port of the ProStar 355 until it bottoms out Hold the needle with one hand and swage the ferrule onto the needle with the 5 16 wrench Remove the needle and assemble it to the syringe 3 Equilibrate the ProStar 355 by pumping deionized water through both reference and sample cells or with the syringe inject deionized water into the two cells ProStar 355 Refractive Index Detector 81 To equilibrate with a pump e Set pump flow rate to 1 mL min e Let flow for 5 minutes e Press Purge flow path will include both sample and reference cells e Let flow for 5 minutes e Press Purge flow path excludes reference cell To equilibrate with a syringe e Fillthe 5 mL syringe with deionized water e Connect the syringe needle t
44. e flow system consisting of pump damper injector column sample and reference cells etc must be primed with the mobile phase Flush the entire system with 5 10 times the system volume until a steady baseline is obtained 3 The mobile phase should be pre mixed and degassed before use Alternately the mobile phase can be degassed online by a solvent degassing system NOTE NEVER try to mix immiscible liquids in your HPLC system If you wish to replace one solvent with an immiscible one flush out the existing mobile phase with an intermediary solvent intermiscible with your initial and final solvents For example you wish to replace water in your HPLC with chloroform water and chloroform are immiscible Replace the water in your system with 2 propanol which is freely miscible with water and chloroform When you are certain all water is removed replace the 2 propanol with chloroform See the Miscibility Chart on page 110 4 If you are using more than one detector in series with the ProStar 355 the RI detector must always be the last component 5 Thecell pressure upper limit is 7 atm 100 psi Use tubing of 0 040 ID or greater on the waste outlet to protect the cells from elevated pressure which could break them Should the cells be damaged the eluate will flow from the DRAIN on the side panel ProStar 355 Refractive Index Detector 49 The cell assembly should only be replaced by a Varian Customer Support Representative C
45. ence mode is Fine 70 85 102195 00 2 OPERATION S Start Up Sequence mode is Standard C Start Up Sequence mode is Coarse INTENS Intensity xxx min Maximum time remaining for the Start Up Sequence Parameter Settings Screen To set the operation parameters 1 From the Monitor Screen press the right arrow key to display the Parameters Screen 2 Usethe Up and Down arrow keys to scroll through the parameters To change a parameter scroll to the appropriate parameter press the Enter key then use the Up and Down arrows to find the desired new setting 3 Once the appropriate new setting is displayed press the Enter key to save the setting You can press the Cancel key to cancel a new setting or the Escape key to return to the Monitor Screen The following table outlines possible operation parameters Parameter Selectable values Unit Default REC RANGE 0 25 0 5 1 2 4 8 16 uRIU 10 mV 512 32 64 128 256 512 12 steps INTEG RANGE 125 500 uRIU 1 V 500 TEMPERATURE 0 30 50 1 step C 35 0 Temp control OFF TIME CONSTANT 0 1 0 25 0 5 1 1 5 2 s 3 3 6 8 steps POLARITY N A BASELINE SHIFT 0 50 1 step 10 mV E S SEQ MODE Fine Standard Coarse Refer to the next table Standard LEAK SENSOR ON OFF N A ON KEY LOCK YES NO N A NO DEFAULT DATA YES NO N A NO ProStar 355 Refractive Index Detector 71 Pre O
46. eratore 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 Leini TO NOTA Sono informazioni utili ad ottenere le prestazioni migliori da parte dello strumento ATTENZIONE Allerta l operatore su situazioni che potrebbero causare ferite leggere e danni limitati allo strumento ed il modo di evitarle ATTENZIONE Allerta l operatore su situazioni potenzialmente pericolose che possono causare danni molto seri ed il modo di evitarle ProStar 355 Refractive Index Detector 29 Segnali di ATTENZIONE ATTENZIONE Pericolo di folgorazioni ATTENZIONE ESPOSIZIONE A SOSTANZA CHIMICHE gt D ATTENZIONE Pericolo di scottature ATTENZIONE PERICOLO PER GLI OCCHI ATTENZIONE Pericolo di incendio f ATTENZIONE ZA Pericolo di esplosioni N ATTENZIONE Pericolo di radiazioni 2 ATTENZIONE Parti in movimento Descrizione del Pericolo Nello strumento sono presenti tensioni pericolose Scollegare il cavo di alimentazione prima di togliere il pannello fissato con le viti Possono essere presenti composti chimici pericolosi Evitare il contatto
47. erheating Low light intensity Null glass home position error Lost parameters Optical balance Capacity lt DC 24 V 0 1 A RS 232C SST316 PTFE Quartz Glass Span Validation guide Physical Specifications Recorder output Integrator output Power requirement Power consumption Dimensions Weight Environment 108 0 10 mV FS 0 1 V FS Sensitivity 2 mV uRIU 8 mV uRIU AC 100 240 V 10 50 60 Hz 150 VA maximum 260 mm W x 150 mm H x 430 mm D a W xb Hx c D 13 kg 27 Ib Your instrument is designed for indoor use only It is suitable for the categories stated on the front of this manual Operation within specifications from 10 to 35 C without failure from 0 to 50 C and non operational storage from 20 to 65 C Operates in relative humidity from 5 to 95 For optimum analytical performance the ambient temperature of the laboratory should be between 20 and 25 C and be held constant to within 2 C throughout the entire working day 85 102195 00 2 APPENDIX Physical Constants of Select Solvents From High Purity Solvent Guide Copyright 1982 Burdick and Jackson Laboratories Inc 1953 South Harvey Street Muskegon Michigan USA 49442 Reprinted with permission of publisher All measurements were made on Burdick amp Jackson solvents at 20 C unless otherwise indicated Listed in order of increasing refractive index Methanol 1 3284 2 Methoxyethyl Acetate 1 4022 Water 1 3330 Cyclopen
48. es tuyaux de raccordement propres sur le plan chromatographique Varian P N 0391832600 et pouvant supporter des pressions sensiblement plus lev es que la plus haute pression de sortie du r gulateur Store and handle compressed gases carefully and in strict adherence to safety codes 85 102195 00 2 INFORMATIONS ET MESURES DE SECURITE Mesures de s curit en CPG Systeme 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 a analyser des substances chimiques dangereuses Lors de l installation de tels conduits m N tiliser 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 l ECD Ni63 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 l ECD Ni63 m Se conformer aux proc dures et au calendrier des essais d tanch it Risque de br lures Les zones des chromatographes gaz chauff es ou trait es cryog niquement peuvent rester tr
49. ex Detector 37 Warnungssymbol WARNUNG ELEKTRISCHER SCHLAG A WARNUNG CHEMISCHE GEFAHR WARNUNG VERBRENNUNGSGEFAHR WARNUNG AUGENVERLETZUNG i WARNUNG FEUERGEFAHR A WARNUNG ZA EXPLOSIONSGEFAHR WARNUNG STRAHLUNGSQUELLE WARNUNG AN BEWEGTE TEILE 38 Warnungsbeschreibung Gef hrliche 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 Kontakt besonders beim Auff llen 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 85 102195 00 2 SICHERHEITSINFORMATIONEN Allgemeine Sicherheitsma nahmen Befolgen Sie diese Sicherheitspraktiken f r eine gefahrlose Ger tebenutzung m Pr fen Sie regelm ig alle Versorgungs u
50. gnal trace is encompassed by the two parallel lines while keeping the vertical distance between these two parallel lines at a minimum Measure the vertical distance between the two parallel lines in each minute segment Convert these values to refractive index units RIU Look at the 20 minutes of noise data and find 15 consecutive minutes of noise when summed together give the smallest total Average these values to find detector noise See below for an example of the ProStar 355 noise measurement 85 minutes of baseline at range 1 4 x 10 RIU FS one minute in length Collect at least 15 Draw parallel lines such that all random variations in that minute are enclosed yet the distance between the lines is minimized See A Convert the distance between the parallel lines into refractive index units Find the mean value of this one minute 1 8 x 10 RIU in this Effect of environment on baseline B was noise over 15 taken in a thermally minutes Noise is stable room C was A measured with the than one hour later same detector less beneath air conditioning vent Figure 14 A Example Noise Test Data of the ProStar 355 Detector 85 102195 00 2 86 OPERATION Figure 19 Band C Example Noise Test Data of the ProStar 355 Detector 87 ProStar 355 Refractive Index Detector Examples Using the ProS
51. h the display When the output appears constant proceed to the next step If the mV output drifts the chromatographic system and or the temperature control have not stabilized Repeat this step until the output remains close to zero and stabilizes Go to the Parameters Setting screen and select the REC RANGE parameter Use the UP or DOWN arrows until the desired sensitivity is reached Turn the recorder on and start the paper Press Zero When the recorder trace goes off scale re zero with the Zero key Monitor the ProStar 355 signal drift i e the rate of change of the signal in RIU hr to see if the instrument and chromatographic system are sufficiently stabilized for the selected sensitivity At a range setting of 1 x 106 RIU FS with water flowing at 1 mL min drift is typically 396 or less of full scale within one hour Higher sensitivities may require more time to achieve this drift 8 Once the desired level of stability is reached press the Purge key to isolate the reference cell from the flow path A single deflection of the pen is expected Because the chromatographic and temperature systems have stabilized baseline restabilization usually occurs rapidly NOTE Tetrahydrofuran THF if not stabilized with antioxidant is an exception The THF in the reference cell will oxidize until a plateau is reached before restabilization occurs 9 At time of sample injection press Marker to mark the moment of in
52. he cabinet Do not lift by knobs or terminals The Varian ProStar 355 weighs 13 kg 27 Ib Use proper lifting techniques to avoid potential injuries ProStar 355 Refractive Index Dectector 47 Do s and Don ts of RI Detectors 1 NEVER subject the reference and sample cells to back pressures greater than 7 atm 100 psi High pressures can break the cells which are difficult to replace NEVER place a backpressure regulator Such as Varian part number 0391939300 on an RI detector Maximum flow cell backpressure is 7 atm 100 psi When placing more than one HPLC detector in series always place the RI detector last Use tubing of 0 040 ID or greater on the waste outlet of the ProStar 355 for less back pressure Locate the ProStar 355 in an area that does not incur large temperature changes The ProStar 355 has a sophisticated temperature control system but care in choosing its operating environment will ensure better operation see Installation Site Requirements page 48 Always pre mix and degas the mobile phase Do not allow pumps to mix solvents for the mobile phase Use only isocratic conditions Keep the RI cells clean See page 93 for the Cell Cleaning Procedure When filling the reference cell ALWAYS use mobile phase that has eluted through the analytical column Allow mobile phase to flow through the column for 10 minutes prior to filling the reference cell Installation Site Requirements Select the inst
53. he front of the optics module behind the front panel underneath the Pre amplifier PC Board see Figure 17 Front Barrier Strip Spade lug connectors ae from lamp and valve occ Solenoid Valve 00 997559 31 Lamp Assembly underneath Pre amplifier Board 03 926028 10 Location of Daughter Boards x Pre amplifier Board 03 926028 02 Optics Module Figure 16 Interior Components of the ProStar 355 96 85 102195 00 2 Outer module cover Urethane foam insulant Inner module cover Flow cell assembly Photodiode assembly Lamp assembly Mirror assembly Mirror assembly screws 2 Flow cells with retainer OONDOOaARWND A Optical unit N PC Board Flow cell retaining screws 2 Mounting Plate for Pre amplifier MAINTENANCE AND TROUBLESHOOTING Figure 17 Optics Module 2 ProStar 355 Refractive Index Detector Test the lamp disconnect the lamp power cable from its terminals Using an ohmmeter measure the resistance across the filament An extremely high or infinite resistance indicates a burned out filament Next reconnect the lamp to its terminals and turn ProStar 355 power on The lamp should have a nominal voltage of 3 V A voltage reading across the lamp filament of 5 V or more indicates a fatigued filament which should be replaced However if neither a burned
54. hoxyethanol 5 0 Carbon Tetrachloride 1 6 b Phenethylamine 5 0 Toluene 2 4 Acetone 5 1 Methyl t Butyl Ether 2 5 Methanol 5 1 o Xylene 2 5 Pyridine 5 3 Benzene 2 7 Diethyl Carbonate 5 5 Chlorobenzene 2 7 2 Methoxyethanol 5 5 o Dichlorobenzene 2 7 Acetonitrile 5 8 Ethyl Ether 2 8 Propylene Carbonate 6 1 Methylene Chloride 3 1 Dimethyl Formamide 6 4 Ethylene Dichloride 3 5 Dimethyl Acetamide 6 5 1 Butanol 3 9 N Methylpyrrolidone 6 7 2 Propanol 3 9 Dimethyl Sulfoxide 7 2 2 Butanol 4 0 Water 10 2 n Butyl Acetate 4 0 Classification of the Solvent Properties of Common Liquids L R Snyder Journal of Chromatography 92 223 1974 Journal of Chromatography Science 16 223 1978 ProStar 355 Refractive Index Detector 111
55. i a luce ultravioletta montano degli schermi di protezione per evitare che gli operatori siano esposti a radiazioni pericolose Per una 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 Disponibilita delle Parti di Ricambio E politica della Varian il fornire le parti di ricambio per lo strumento ed i suoi accessori per un periodo di cinque 5 anni a partire dalla data di produzione dell ultima 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 produzione dell ultima unit delle serie solo in base alla loro disponibilit Servizi Tecnico La Varian alla scade
56. ic or other machine readable form in whole or in part First published February 2005 in Australia preliminary edition Updated in May and August 2005 Comments about this manual should be directed to the Marketing Communications Manager Varian Australia at the address above or by e mail to osi_webmaster varianinc com Varian Australia is ISO9001 2000 certified 2005 Varian Australia Pty Ltd A B N 67 004 559 540 All rights reserved ERC INC R006 Rev 0 DECLARATION OF CONFORMITY Suppliers Name ERC Inc Suppliers Address 5 8 6 Nishi Aoki Kawaguchi City Saitama 332 0035 Japan Declares that the product Product Name Refractive Index Detector Model Number s ProStar 355 Conforms to the following product specifications Safety IEC 61010 1 2001 Second edition EN 61010 1 2001 Second edition Safety requirements for electrical equipment for measurement control and laboratory use Part 1 General requirements EMC EN 61326 1997 Al 1998 A2 2001 EMC requirements for electrical equipment for measurement control and laboratory use Part 1 General requirements 1 EMI CISPR 11 1997 CISPR 14 1 2000 CISPR 16 1 1999 CISPR 16 2 1996 CISPR 22 1997 TEC 61000 3 2 2000 IEC 61000 3 3 1995 2 EMS IEC 61000 4 2 1995 IEC 61000 4 3 1995 IEC61000 4 4 1995 IEC 61000 4 5 1995 IEC 61000 4 6 1996 IEC61000 4 8 1993 IEC 61000 4 11 1994 Location Table of Contents Safety
57. ills can occur when conductive HPLC solvents are spilled on or in the instrument Ground the instrument properly to protect the operator from electrical shock Proper grounding also protects the instrument from power line noise Verify that the instrument is properly grounded through the power line ground terminal Do not remove or otherwise disable the power cord s ground prong Preparing the ProStar 355 for Operation The ProStar 355 as delivered is not ready for operation The following three steps must first be performed e Install the fuse and power cable e Loosen the shipping bolts e Install the drain tube Installing the fuse and power cable The instrument is shipped without a power cable or fuse installed Install as follows 1 Check that the power is OFF WARNING FIRE HAZARD Replace only with same type and rating of fuse 2 Confirm that the voltage of the power socket into which the ProStar 355 will be plugged is the same as the voltage indicated on the rear panel of the detector Install the supplied fuse 4 Ensure that the power is OFF and connect the appropriate power cord 52 85 102195 00 2 INSTALLATION WARNING SHOCK HAZARD Prior to connection ensure that the voltage of the power socket into which the detector power cable is being plugged is the same as the power supply voltage indicated on the detector The power socket should be of a three pin type with a grounding terminal Do not use other
58. irst the digital signal recorder or integrator output display should be near zero Second all lighted indicators should be green A yellow LED indicates Caution the ProStar 355 is not ready for injection During analysis the digital signal display may move up scale or sometimes down scale indicating the passage of compounds through the sample cell This is a normal operating characteristic During a long run at high sensitivity the baseline may drift slightly This may be due to a temperature change or change in the composition of one or both liquid cells oxidation dissolved gas solvent impurities column ProStar 355 Refractive Index Detector 75 bleeding etc If such drift is tolerably slow continuous compensation can be made by repeating the zero adjustment procedures but only during periods when no sample peaks are passing through the detector Familiarization Exercise The following procedure demonstrates the operating characteristics of the ProStar 355 controls and shows the effects of the controls on the recorder and integrator output signals 1 76 The ProStar 355 should be filled with water thermostatted equilibrated and zeroed Refer to steps 1 7 in Recorder Output on page 72 Set the REC RANGE to 1x10 RIU if a chart recorder is in use If an integrator data system is in use find an attenuation setting that gives about the same signal amplitude for your recorder and integrator Fo
59. is measured Zero refraction should give a zero volt difference in these signals An electrically controlled mechanical linkage allows the user to optimize the photodiodes outputs for zero deflection via a refractive lens in the optical path Additional circuitry enables the user to easily correct the signal output to electronic zero When a change occurs in the refractive index of the mobile phase the light passing through the interface between the sample and reference cells is refracted causing the light intensity on one photodiode to increase and on the other to decrease This difference gives a signal having both amplitude and polarity the signal is amplified to drive a chart recorder or digital integrator One difficulty with refractive index detection in HPLC is that the refractive index of a liquid is a function of temperature Temperature variation of the mobile phase at the point of measurement produces signal drift and noise The ProStar 355 minimizes this problem by active thermostatting of its optics module combined with efficient heat exchange technology and temperature monitoring feedback As a result the flowing mobile phase is always well equilibrated at the operating temperature The ProStar 355 has external connections on its rear panel for contact closure operation by a data system instrument controller autosampler or other external device Any device or instrument that can supply a contact closure can purge the ProS
60. jection 85 102195 00 2 OPERATION Integrator Output 1 Perform steps 1 through 4 of Recorder Output on page 72 2 Setthe integrator or data system to the desired attenuation Press Zero on the ProStar 355 to begin monitoring the signal 3 Monitor the ProStar 355 signal drift i e the rate of change of the signal in RIU hr until the instrument and chromatographic system are sufficiently stabilized to use at your desired attenuation NOTE Many integrators and data systems have mechanisms to correct for signal offsets at time zero For this reason it is advisable to Auto Zero the ProStar 355 prior to monitoring the signal on the integrator or data system Otherwise signal zero may be off scale on the integrator 4 Once the desired level of stability is reached press the Purge key to isolate the reference cell from the flow path A signal deflection of the pen due to a pressure differential between reference and sample cells is to be expected Press Zero Because the chromatographic and temperature systems have stabilized once already restabilization usually occurs rapidly NOTE Tetrahydrofuran THF if not stabilized with an antioxidant is an exception THF in the reference cell will oxidize until a plateau is reached before restabilization occurs The ProStar 355 is now ready for injection Routine Operation The ProStar 355 Refractive Index Detector should indicate to the user that it is ready for operation F
61. 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 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 All components of the system should be connected to a common power supply and common ground This ground must be a true ground rather than a floating ground Non polar solvents can develop a static charge when pumped through the system All vessels that contain mobile phase including tubing and collection vessels must be grounded to dissipate static electricity Employ static measuring and static discharge devices e g air ionizers to safeguard against the buildup of static electricity 8 85 102195 00 2 SAFETY INFORMATION Ultraviolet Radiation Liquid chromatograph detectors that use an ultraviolet light source have shielding to prevent radiation exposure to personnel A WARNING EYE HAZARD For continued protection m Ensure that protective lamp covers of variable and fixed wavelength detectors are in place during operation m
62. manutenzione routinaria del sistema m Non smontare mai una linea del solvente od una valvola quando il sistema amp 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 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 solventi non polari possono sviluppare una carica statica quando vengono pompati attraverso il sistema Tutti i recipienti che contengono la fase mobile inclusi i tubi e i recipienti di raccolta devono avere una messa a terra per disperdere l elettricit statica Vanno utilizzati dispositivi di misurazione e scarico ad esempio ionizzatori d aria per evitare l aumento di elettricit statica 34 85 102195 00 2 INFORMAZIONI SULLA SICUREZZA Radiazioni Ultraviolette rivelatori di cromatografia liquida che usano sorgent
63. mated and manual high performance liquid chromatography The ProStar 355 is a deflection or Snell type refractive index detector Snell s law states that a parallel light beam when passing through a dielectric interface separating two media of different refractive index at an angle of incidence greater than zero will be refracted as a function of the magnitude of difference of the refractive indices of the two media See figure below interface n index of refraction i angle of incidence r angle of refraction refracted beam v velocity of light in first medium v velocity of light in second medium where Figure 1 Snell s Law ProStar 355 Refractive Index Detector 45 46 Light from a low power long lifetime tungsten lamp is collimated by a lens and slit and passed through reference and sample cells reflected off a mirror passed back through the optical cells and focused by lenses onto a pair of photosensing diodes During operation the ProStar 355 reference and sample cells are filled with mobile phase The reference cell is then isolated from the flow path and mobile phase flows through the sample cell only As long as no difference exists between the refractive indices of the media of the two cells there is no refraction of the light passing through them The light shines on a pair of photodiodes each of which gives an electrical signal these signals are amplified and the difference in the two signals
64. me Temperature control Flow cell volume Maximum flow rate Pressure rating Internal volume Deflection 1 00 1 75 RIU ato 512 x 10 RIU FS 2 5 x 10 RIU Response 1 5 s 600 uRIU 0 1 0 25 0 5 1 0 1 5 2 3 6s OFF 30 50 C 1 C increment 77 C fuse 8 uL 10 mL min mobile phase pure water 50 kPa 0 5 kgf cm Inlet port Flow cell approx 60 uL Flow cell Outlet port approx 520 uL Total approx 590 uL General Specifications Auto zero Auto zero range Auto zero resolution Offset range Electrical and optical zeroing All refractive index ranges lt 1 E 2 mV yRIU 4 8 mV uRIU nRIU 0 500 mV Integrator output 0 50 Recorder output ProStar 355 Refractive Index Detector 107 Offset resolution Event marker Reference cell purge Polarity External signal input contact closure Signal output contact closure External communication Wetted material Operator support 10 mV same with Integrator output sensitivity Marker out 5 of FS Flow of mobile phase through a reference cell is controlled by the front panel PURGE key When activated a solenoid switch places both the reference and sample cell in line with the mobile phase Each momentary contact closure switches the event to its opposite state ON to OFF positive to negative Auto Zero Marker Purge On Off 1 Ready 2 Solvent leak 3 Error one of the following errors has occurred Ov
65. ment CAUTION Alerts you to situations that may cause moderate injury and or equipment damage and how to avoid these situations WARNING Alerts you to potentially hazardous situations that could result in serious injury and how to avoid these situations Warnings are accompanied by a triangular symbol indicating the type of warning ProStar 355 Refractive Index Detector Warning Symbol Warning Description Hazardous voltages are present inside instrument ae Disconnect from main power before removing screw SHO attached panels WARNING Hazardous chemicals may be present Avoid contact CHEMICAL HAZARD especially when replenishing reservoirs Use proper eye and skin protection WARNING BURN HAZARD Very hot or cryogenically cold surfaces may be exposed Use proper skin protection WARNING EYE HAZARD Eye damage could occur either from flying particles chemicals or UV radiation Use proper eye and face protection Ia WARNING FIRE HAZARD The potential for fire may be present Follow manual instructions for safe operation ty WARNING lA ZX EXPLOSION HAZARD The potential for explosion may exist because of type of gas or liquid used WARNING RADIATION SOURCE lonizing radiation source is present Follow manual instructions for safe operation WARNING MOVING PARTS Keep hands and fingers away WARNING HEAVY WEIGHT A A heavy object is present Avoi
66. n Stromquellen bevor Sie Schutzpaneele entfernen damit Sie nicht mit potentiell gef hrlichen Spannungen in Ber hrung kommen m 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 m Ersetzen Sie durchgebrannte Sicherungen nur mit Sicherungen der Werte die am Sicherungspaneel oder im Handbuch angegeben sind m Ersetzen Sie fehlerhafte oder durchgescheuerte Netzkabel sofort durch Kabel gleicher Art m Sorgen Sie daf r da Spannungsquellen und die Netzspannung den gleichen Wert haben f r den das Instrument verdrahtet ist Gasdruckflaschen m Lagern und handhaben Sie komprimierte Gase vorsichtig und in strikter Einhaltung der Sicherheitsvorschriften m Befestigen Sie die Gasflaschen an feststehenden Aufbauten oder an W nden m Lagern und transportieren Sie Gasflaschen in aufrechter Stellung Druckregler zuvor abnehmen m Lagern Sie Gasflaschen in gut durchl fteten R umen weit genug weg von Heizungen direktem Sonnenschein Frosttemperaturen und Entz ndungszonen m Kennzeichnen Sie die Flaschen so eindeutig da kein Zweifel ber deren Inhalt bestehen kann m Benutzen Sie nur gepr fte Druckminderer und Verbindungsst cke m Benutzen Sie nur chromatographisch reines Verbindungsrohr Varian part 40 number 0391832600 das wesentlich h heren Druck als den h chsten Au
67. nal Circuit Diagram 85 102195 00 2 OPERATION Front panel controls Figure 10 shows the front panel controls on the ProStar 355 ma Leak Di 5 Seq Zero gt Y Purge Marker Escape Cancel Power ProStar pa AR VARIAN amp Power key Power Figure 10 Front Panel Controls Turns the unit ON or OFF LCD Leak LED Leak Liquid Crystal Display This light is illuminated when a solvent leak is detected Start Up Sequence key S Seq Purge key Purge Initiates a Start Up Sequence Turns the purge valve on or off in order to change the flow path When the valve is on the PURGE sign is highlighted with a yellow background and solvent flows through the reference side of the flow cell instead of the sample side Press the Purge key again to turn off the valve The Purge key is not functional during the Start Up Sequence Auto Zero key Zero Marker key Marker Activates an Auto Zero The Zero key does not function during a sequence Generates an event marker signal i e a momentary voltage spike is put on top of the recorder output 10 of Full Scale ProStar 355 Refractive Index Detector 69 Arrow keys These keys move the cursor in the LCD and enable you to edit values By default the cursor will scroll in a circular motion Escape key Escape Returns the LCD display to the Monitor Screen Cancel key Cancel Cancels an edited value in
68. nd Pneumatikleitungen auf Lecks m Gasleitungen d rfen nicht geknickt oder angestochen werden Verlegen Sie die Leitungen au erhalb von Laufwegen und abseits von extremer Hitze oder K lte m 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 m Sammeln Sie keine L sungsmittelabf lle Entsorgen Sie solche Materialien ber ein geregeltes Entsorgungsprogramm und nicht ber die ffentlichen Abwasserleitungen HINWEIS WARNUNG WARNUNG Dies Instrument 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 Dies Instrument ist f r chromatographische Analysen entsprechend pr parierter Proben gedacht Es mu mit geeigneten Gasen und oder L sungsmitteln und innerhalb der im Handbuch 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 Kundendienstvertreter zu informieren wenn das Instrument f r Analysen gef hrlicher biologischer radioaktiver oder toxischer Proben benutzt worden ist ProStar 355 Refractive Index Detector 39 Elektrische Gefahren m L sen Sie das Instrument von alle
69. nstrucciones de Operacion Este Manual de Instrucciones esta 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 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 PRECAUCION Le alerta de situaci nes que pueden causar da os moderados a la salud 6 al equipo y c m evitar esas situaciones ATENCION Le alerta de potenciales situaciones peligrosas que pueden causar serios da os y c mo evitar esas situaciones ProStar 355 Refractive Index Detector 13 Simbolo ATENCION PELIGRO DE g DESCARGA ELECTRICA ATENCI N PELIGRO QU MICO ATENCI N PELIGRO DE QUEMADURAS ATENCI N PELIGRO PARA LOS OJOS gt ATENCION PELIGRO DE FUEGO ATENCION ZX PELIGRO DE EXPLOSI N PA ATENCI N PELIGRO DE RADIACION A ATENCION PARTES EN MOVIMIENTO 14 Descripcion El instrumento utiliza voltages peligrosos Desconecte el interruptor general antes de retirar los paneles atornillados Peligro de productos quimicos Evite el con
70. nt that contains halogens such as chloroform and methylene chloride has been used flush out all lines with a solvent compatible with your chromatographic conditions and column For example hexane or another hydrocarbon For isocratic work with a 85 102195 00 2 OPERATION normal phase column the alcohols methanol or 2 propanol a non carcinogenic aromatic such as the xylenes acetone or an ether that is non volatile and not a ready producer of peroxides can be used DO NOT use ethyl ether NOTE Ethanol stabilized chloroform does not form chloride ions readily therefore it is recommended in place of pure chloroform Fluorocarbon solvents will alter PTFE over long exposure Flush with pentane or another light hydrocarbon Limitations in addition to those listed in Table 1 may exist for a specific column Always refer to the column instruction manual for recommendations on solvent limitations If the detector is to be exposed to sub freezing temperatures an antifreeze flush such as methanol must be used General Recommendations for Solvent Preparation Grade of Solvents Solvent Filtering HPLC grade solvents are recommended for better instrument performance and chromatographic data Solvents that are easily oxidized e g Tetrahydrofuran THF require the addition of an anti oxidant Anti oxidants however will not affect refractive index data THF when used as an isocratic mobile phase in GPC Gel Permeation
71. nza 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 mente 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 ProStar 355 Refractive Index Detector 35 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 36 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
72. o only 700 kPa 7 atm Gently flush the cells under all conditions If you encounter a large backpressure in the ProStar 355 proceed cautiously You will be risking cell rupture and cell assemblies should only be replaced by Varian Customer Support Representatives Cell Cleaning Hints The following recommendations may be applicable to a variety of cleaning conditions 1 Clean all internal lines of the ProStar 355 by injecting cleaning solution with Purge off and inject cleaning solution again with Purge on ProStar 355 Refractive Index Detector 93 2 Particulate matter can be removed by forcing liquid through the cell using the syringe and needle with tubing from your Accessory Kit Sometimes it helps to reverse flow and inject in the OUT port If liquid purging does not work try gas purging Replace cell liquid with a volatile e g acetone solvent Purge and dry the cells with clean gas at about 50 psi Gas flowing through the cell will sometimes dislodge particles Also try reversing the flow direction For difficult entrapments follow the above gas purge procedure with a liquid purge When liquid hits a particle in a dry cell it is generally more effective than a continuous liquid purge 3 If you suspect that you have a problem with entrapped bubbles purge with 2 propanol 4 Heating the flow cells may remove marginally soluble material Acid Cleaning WARNING lA CHEMICAL HAZARD Corrosive acids are used Use ex
73. o 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 frecuencias que no est n incluidas dentro de los l mites testados Este instrumento est dise ado para an lisis cromatogr fico de muestras preparadas apropiadamente Debe ser operado usando gases y disolventes apropiados y con unos niveles m ximos de presi n flujos y temperaturas seg n se describe en este manual 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 ProStar 355 Refractive Index Detector 15 Peligros Electricos 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 con fusibles del tipo y tamafio 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 la
74. o the IN port of the ProStar 355 e Press Purge flow path will include both sample and reference cells e inject 4 5 mL of water into the IN port NOTES Itis normal to feel considerable backpressure on the syringe A 1 3 mL syringe Varian part number 0099672118 can be used in place of the 5 mL syringe for less pressure Complete the noise and drift measurements with the pump off Elevating the waste container above this detector will help eliminate drift by preventing siphoning of mobile phase from the flowcell 4 When the detector has stabilized turn the Purge off to isolate the reference cell from the flow path Press Zero to adjust signal zero to recorder zero Monitor the signal to verify that output is approximately zero and remains stable DRIFT 5 Setthe REC RANGE to 1x10 RIU 6 Turn pump flow off and disconnect the inlet line from the detector if you equilibrated the detector with an HPLC pump If you injected the deionized water into the cells with the needle the needle can remain in the inlet 7 Record thirty minutes of baseline Draw two parallel lines in such a way that the entire thirty minutes of baseline is encompassed by the two parallel lines while keeping the vertical distance between these two parallel lines at a minimum Refer to Figure 13 82 85 102195 00 2 ProStar 355 Refractive Index Detector OPERATION Calculate the slope of either line in refractive index units per hour RIU hr
75. ock Diagram and Basic Circuitry of the ProStar 355 67 Front parnel Controls teo alae Alas t ue Anne 69 Pre Operation Check LISL latin edt ee He e en dani trie eds 72 Instrument Operation sise 72 Starting up using Start Up Sequence ii 72 Stand Up MANUAI s ss 2 re tera repeat nr IP metier I RAF ete annee Nes ESSERE 73 Routine Operationen anna e aa aai eae EEA a E E OSEE E 75 Familiarization Exercise iced de end eed nn 76 ProStar 355 Refractive Index Detector i Calibrating and Testing the ProStar 355 77 Validation Display Screen 77 Noise and Drift Testi nee 81 Examples Using the ProStar 355 us 88 Manual Mode i ner t ete ceteri tata 88 Shutdown Procedures ire teet pep n o en hi ente vip pines 90 Corrosive SOlvents e itera e rf o idi prod edad cea ded caede pe use 90 No Flow Versus Reduced Flow sese nennen 90 Continuous Power On Versus Power Off 91 LongsTerm Storage ted eee nuu eiae 91 Maintenance and Troubleshooting uurssssnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn 93 Cell Cleaning Procedure iii 93 Preparation for Cell Cleaning sese 93 Gell Cleaning Elite ii 2 ee t eee Eo vc tete 93 Acid Cleaning s roo eterne een tt ete len assiale eni 94 Other Cell Cleaning Procedures nn 95 Lamp Replacement and Adjustment sess eene nennen 95 Lamp Removal and Replacement
76. onduits de gaz l cart des all es et venues et l abri du chaud ou du froid m 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 m 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 ATTENTION ATTENTION 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 congu pour effectuer des analyses chromatographiques d chantillons pr par s selon des m thodes appropri es Il convient de le faire fonctionner avec les gaz et ou les solvants ad quats et dans les limites des pressions des d bits et des temp ratures 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 a t utilis pour l analyse d chantillons biologiques dangereux radioactifs ou toxiques avant que n en soit effectu la maintenance ProStar 355 Refractive Index Detector 23 Risques de chocs electriques D connecter le mat riel de toute source d alimen
77. or HPLC systems Generally however the rule of thumb is to add one component at a time back into the HPLC system so that should the condition arise again the component causing the problem is indicated You will begin by adding the pump to the ProStar 355 first and you will add the column last If another type of detector is available itis advantageous to use it before the ProStar 355 to aid in troubleshooting Example you have a UV detector before the ProStar 355 and only the ProStar 355 has a noisy baseline One possible implication is that the noise arises from pressure fluctuation to which the refractive index detector is more sensitive On the other hand if both detectors are showing noise a power line current may be indicated If both detectors show anomalous baseline performance such as huge peaks that continue indefinitely a bleed off problem material from the column or immiscible solvents trapped in the system is more likely ProStar 355 Refractive Index Detector 103 Troubleshooting Table For further assistance phone 1 800 FOR HPLC or contact your local Varian office Cause Bubble in the pump Problem Noise Bubble in the detector Dirty flow cell s Weak lamp Environmental temperature fluctuations Vapor pressure of the mobile phase is too high for the detector Example of difficult solvents above 30 C Acetone cyclopentane methyl t butyl ether trichlorotrifluoroethane pentane di
78. ove 30 C Acetone cyclopentane methyl t butyl ether trichlorotrifluoroethane pentane dichloromethane ethyl ether and many fluorocarbons Tetrahydrofuran THF in the mobile phase will oxidize in the reference cell Reference cell solvent has aged and deteriorated Sample and reference cells do not contain identical solutions Reference cell contains air bubbles Flow cell s dirty Deteriorating lamp or lamp out of adjustment Lamp is burned out Flow cell s dirty Reduce or turn temperature the temperature off Cool mobile phase column and detector Modify method to exclude or decrease concentration of troublesome solvent Add an antioxidant to stabilize the THF if compatible with other chromatographic requirements Allow 2 hours stabilization time for oxidation in reference cell to reach a steady state condition Flush reference cell with mobile phase Flush sample and reference cells with mobile phase Flush sample and reference cells with mobile phase Clean flow cell Refer to Cell Cleaning procedure on page 93 Test lamp and replace or adjust as necessary Refer to the Lamp Test procedure on page 95 Test lamp and replace or adjust as necessary Clean flow cell Refer to Cell Cleaning procedure on page 93 85 102195 00 2 Appendix Specifications Performance Specifications Detector type Refractive index range Range Noise Linearity Response ti
79. peration Check List Before operation check the following detector and system connections and switches Shipping bolts loosened per Loosening the Shipping Bolts on page 53 Desired analytical column installed Mobile phase flushed through all of the HPLC system all incompatible or immiscible solvents have been flushed out see page 48 Connections made to chart recorder integrator data system or other external equipment see page 59 and page 60 All tubing connections are made and checked for leaks see page 55 Power socket voltage matches voltage indicated on rear panel see page 52 Drain tube is installed see page 54 Detector pump and peripherals are plugged into appropriate power receptacles Power switches on the pump peripherals and other detectors are ON Instrument Operation Starting up using Start Up Sequence 72 To perform an unattended start up 1 Set the operating parameters using the Parameter Settings Screen 2 Start pumping mobile phase solvent at a flow rate of 1 mL min 3 Press the S Seq key to initiate the Start Up Sequence 85 102195 00 2 OPERATION The following table shows fixed values for the Start Up Sequence Parameter Fine Purge Cycle Number of Cycles Time to Auto Zero Standard Default Coarse 30s 3 240s Equilibration Time 60 min 40 min Measuring Time 60 min 40 min Drift 100 nRIU h 500 nRIU h 2500 nRIU h Noise 4 50 nRIU If drift or noi
80. quipment is used in a manner not specified by the manufacturer the protection provided by the WARNING equipment may be impaired fa EYE HAZARD WARNING It is the responsibility of the Customer to inform Varian CHEMICAL HAZARD Customer Support Representatives if the instrument has been used for the analysis of hazardous biological radioactive or toxic samples before any instrument service being performed or when an instrument is being returned to the Service Center for repair 4 85 102195 00 2 SAFETY INFORMATION Electrical Hazards WARNING SHOCK HAZARD ProStar 355 Refractive Index Detector Disconnect the instrument from all power sources before removing protective panels to avoid exposure to potentially dangerous voltages Panels or covers which are retained by screws on the detector may be opened ONLY by Varian trained Varian qualified or Varian approved Customer Service Representatives Consult the manuals or product labels supplied with your PC to determine which parts are operator accessible 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 Good grounding earthing is essential to avoid a potentially serious electric shock hazard Ensure that there is an integral ground connection between the metal base of the detector and the 3 pin earth grounded receptacle Consult the manuals o
81. r Varian data systems start with attenuation 64 Press the Zero key to re zero the electronics and optics of the ProStar 355 You will oserve that both recorder and integrator signals are affected by these controls Auto Zero is slightly displaced from your recorder zero however this displacement is fairly constant from re zeroing to re zeroing Press Purge to place both the reference and sample cells in line with the mobile phase The resulting change may or may not be significant eough to observe as an output signal All analyses sould be performed with the purge OFF Press the Marker key You will notice that only the recorder output is affected A momentary voltage spike is inserted on top of the recorder outout 85 102195 00 2 OPERATION Calibrating and Testing the ProStar 355 Validation Display Screen The Validation Display Screen allows you to verify that your ProStar 335 hardware is functioning properly You can view e Temperature If the temperature is at the specified temperature 1 C GOOD will be displayed If the temperature is outside this range NG will be displayed e Source lamp voltage If the source lamp voltage is under 4 5 V GOOD will be displayed Otherwise NG will be displayed e Drift and Noise If drift and noise values are under the fixed values in the Start up Sequence GOOD will be displayed Otherwise NG will be displayed e Span If the span is 512 25 uRIU GOOD will be displayed
82. r product labels supplied with your PC for the relevant grounding requirements Replace blown fuses with fuses of the size and rating shown on the fuse panel or in the manual Replace faulty or frayed power cords immediately with the same type and rating Make sure that voltage sources and line voltage match the value for which the instrument is wired Avoid using power supplies from a source that may be subject to electrical or RF interface from other services for example large electrical motors elevators and welders Compressed Gas Cylinders m Store and handle compressed gases carefully and in strict adherence to safety codes m Secure cylinders to an immovable structure or wall m Store and move cylinders in an upright vertical position Before transport remove regulators and install cylinder cap m Store cylinders in a well ventilated area away from heat direct sunshine freezing temperatures and ignition sources m Mark cylinders clearly so there is no doubt as to their contents m Use only approved regulators and connections m Use only connector tubing that is chromatographically clean Varian part number 0391832600 and has a pressure rating significantly greater than the highest outlet pressure from the regulator 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 WARNING
83. ra cualquier consulta sobre Instrumentaci n Analitica 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 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 20 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 A VARIAN www varianinc com 85 102195 00 2 INFORMATIONS ET MESURES DE SECURITE Informations et mesures de securite Instruction
84. s de fonctionnement Ce manuel d instruction est concu 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 meilleur parti du mat riel sur le plan des performances MISE EN GARDE Attire l attention sur une situation pouvant occasionner des dommages corporels l gers et ou des deg ts mineurs l appareil et indique comment rem dier cette situation ADVERTISSEMENT Attire l attention sur une situation potentiellement dangereuse pouvant occasionner des dommages corporels importants et indique comment rem dier cette situation ProStar 355 Refractive Index Detector 21 Symboles d avertissement ATTENTION RISQUE D ELECTROCUTION ATTENTION SUBSTANCES CHIMIQUES DANGER ATTENTION RISQUE DE BRULURES A ATTENTION fa DANGER POUR LES YEUX ATTENTION RISQUE D INCENDIE A ATTENTION AA RISQUE D EXPLOSION A ATTENTION SOURCE DE RADIATION A ATTENTION PIECES EN MOUVEMENT 22 Descrip
85. s l neas de electricidad se ajustan a los valores para los que el Instrumento ha sido preparado Botellas de Gas Comprimido 16 Guarde y maneje las botellas de gas con cuidado y de acuerdo con las normas de seguridad Asegure las botellas a una estructura inmovil 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 limpios Varian p n 0391832600 y que tengan una graduaci n de presi n significativamente mayor que la mayor presi n del regulador 85 102195 00 2 INSTRUCCIONES DE SEGURIDAD 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 quimicas 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 vibraci 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
86. se did not meet target values within a defined period FAIL will be displayed on the Start Up Sequence status line Press the S Seq key to re do the sequence You can press Enter or Cancel to abort the sequence When drift and noise meet the target values within the time limit the sequence is finished and READY will be displayed on the Start Up Sequence status line The ProStar 355 is now ready for injection Starting up manually Recorder Output The ProStar 355 and all peripheral instruments should be plugged in Press the ProStar 355 Power button and set the temperature to the desired temperature using the Parameters Setting Screen The detector will be operational in one to three hours for most applications However at the highest sensitivities up to 24 hours may be needed for stabilization NOTES Ifthe LCD displays TEMP UNSTABILIZE the ProStar 355 cell is not at temperature This message will disappear temperature stabilization is complete Before activating the purge valve LED light OFF pump about 10 mL of liquid through the cell This will flush possible dust or particulate matter and reduce the possibility of damaging the valve seals ProStar 355 Refractive Index Detector 73 NOTE Press the Purge key and pump mobile phase through the sample and reference cells at 1 mL min for approximately 20 minutes The digital output display may or may not be at zero 000 mV at this time Press the Zero key Watc
87. sgangsdruck des Druckminderers aush lt 85 102195 00 2 SICHERHEITSINFORMATIONEN GC Sicherheitspraktiken Abgassystem F r GC Detektoren die in einem gut durchl fteten Raum installiert sind ist keine spezielle Abgasf hrung erforderlich au er 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 Ersch tterungen oder Luftstr mungen nicht die Detektorfunktion beeintr chtigen m Pr fen Sie regelm ig die einwandfreie Arbeitsweise der 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 Ni63 ECD Handbuch m F hren Sie die Tests f r zu beseitigende radioaktive Kontamination durch die im Ni63 ECD Handbuch beschrieben sind m Erf llen Sie die Zeitpl ne und Verfahren zur Dichtigkeitspr fung Verbrennungsgefahr Beheizte oder tieftemperaturgek hlte Zonen des Gaschromatographen k nnen betr chtlich lange hei oder kalt bleiben nachdem das Instrument bereits abgeschaltet 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 benutzen bevor Sie m glicherweise
88. so shows the standards to which the product was tested to demonstrate compliance It is also signed by Varian s Authorized Representative in the EU and by the representative of the manufacturing plant 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 basis after the final production run of the instrument 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 10 85 102195 00 2 Varian Inc Analytical Instruments Sales Offices SAFE
89. sory The following is a Federal Communications Commission advisory CAUTION This equipment has been tested and found to comply with the limits for a Class B digital device pursuant to part 15 of the FCC Rules These limits are designed to provide reasonable protection against harmful interference in a residential installation This equipment generates uses and can radiate radio frequency energy and if not installed and used in accordance with the instructions may cause harmful interference to radio communications However there is no guarantee that interference will not occur in a particular installation If this equipment does cause harmful interference to radio or television reception which can be determined by turning the equipment off and on the user is encouraged to try to correct the interference by one or more of the following measures Reorient or relocate the receiving antenna Increase the separation between the equipment and receiver Connect the equipment into an outlet on a circuit different from that to which the receiver is connected Consult the dealer or an experienced radio TV technician for help WARNING This instrument is designed for chromatographic PA EXPLOSION HAZARD analysis of appropriately prepared samples lt must be operated using appropriate gases and or solvents and within specified maximum ranges for pressure flows HN WARNING and temperatures as described in this manual If the FIRE HAZARD e
90. sts should be made using pieces of 316 stainless steel column tube ferrule etc under these conditions 1 when the solvent to be used is close to the boundary indicated in Table 1 2 when a mixture of solvents is to be used and 3 when the solvent contains some active solutes other than those listed 64 Table 1 Solvent Limitation Recommendations Unusable _ Usable Below 10 Usable Below 30 Usable Below 50 Hydrohalogenic Sulfuric Acid Citric Acid Acetic Acid Acids HCl HF etc Boric Acid NaOH Lactic Acid Metal Halides gt 2M Acetic Anhydride Ammonium salts Hydrazine KCI KOH citrate Ammonium nitrate Ammonium Halides Ammonium salts oxalate K2CO3 Ammonium Formate formate sulfate Sodium formate All hypochlorites perchlorate HoPO4 Tetrachloromethane HPO4 K Na salts of bicarbonate chlorate nitrite If a limited condition solvent listed above is in use flush out all hydraulic lines sufficiently with an inert solvent that is compatible with your chromatographic system and column Buffers acids and other highly ionic aqueous solutions should be flushed out with large amounts of water 5 10 times the volume of liquid from pump head to detector outlet Under some circumstances you may want to follow this deionized water flush with a flush of 2 propanol if it is compatible with the column packing If you neglect this flushing the pump injector and column may become corroded and badly damaged When an organic solve
91. sure at which its performance is poor Drift Detector not yet thermally stabilized Flow cell s dirty Flow cell s damaged Contamination from HPLC System MAINTENANCE AND TROUBLESHOOTING Solution Continuously sparge the mobile phase with helium Move the detector to a more stable environment Place a cover over the detector Flush detector by turning the Purge on and off Verify that correct exit line is installed Inspect exit line for crimps Add a second damper Add a restrictor coil between pump and injector valve Monitor output signal 1 2 hours at 30 C or overnight until stability is reached Clean references and sample cells Refer to Cell Cleaning procedure on page 93 Check for liquid in rear drain tube indicating a broken cell Test cell integrity Refer to Cell Integrity Test procedure on page 100 Flush HPLC system with a solvent stronger than the mobile phase less polar for reverse phase more polar for normal phase etc until contaminant disappears Contaminated or non HPLC grade solvents ProStar 355 Refractive Index Detector Prepare fresh mobile phase premixed degassed 105 Problem Baseline drift starts after several hours of analysis Baseline will not zero Intensity Alarm Lights 106 Vapor pressure of mobile phase is too high for operating temperature causing bubble formation in reference cell Example of difficult solvents ab
92. tacto especialmente cuando rellene los dep sitos Utilice protecci n de ojos y piel Superficies posiblemente calientes 6 frias criog nico Utilice protecci n para la piel Las particulas volatiles productos quimicos o radiaci n UV pueden causar dafos 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 6 liquido 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 85 102195 00 2 INSTRUCCIONES DE SEGURIDAD Precauciones Generales de Seguridad Siga estas indicaciones de seguridad para una correcta operaci n del equipo m Realice verificaciones peri dicas de fugas en todas las l neas de suministro y tuber as m No permita que las l neas de gas se doblen pinchen Mant ngalas alejadas de zonas de paso y del calor 6 fr o excesivo m Guarde los disolventes org nicos en cabinas ventiladas a prueba de fuego y etiquetadas para que puedan ser f cilmente identificadas como material t xico y inflamable m 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 ATENCION ATENCION Este instrumento ha sid
93. tane 1 4064 Acetonitrile 1 3441 Methyl Isoamyl Ketone 1 4070 Ethyl Ether 1 3524 Tetrahydrofuran 1 4072 Trichlorotrifluoro ethane 25 C 1 3557 2 Ethoxyethanol 1 4077 Pentane 1 3575 Propylene Carbonate 1 4210 Acetone 1 3587 Dioxane 1 4224 Petroleum Ether 1 3650 Methylene Chloride 1 4241 Methylt Butyl Ether 1 3689 Cyclohexane 1 4262 Ethyl Acetate 1 3724 Dimethyl Formamide 1 4305 Iso hexanes 1 3740 Isopropyl Myristate 1 4332 Hexane 1 3749 Hexadecane 1 4340 2 Propanol 1 3772 Dimethyl Acetamide 1 4384 Methyl Ethyl Ketone 1 3788 Ethylene Dichloride 1 4448 Glyme 1 3796 Chloroform 1 4458 Diethyl Carbonate 1 3846 Carbon Tetrachloride 1 4601 1 Propanol 1 3856 N Methylpyrrolidone 1 4700 Heptane 1 3876 Decahydronaphthalene 1 4751 Methyl n Propyl Ketone 1 3901 Trichloroethylene 1 4767 Trimethylpentane 1 3914 Dimethyl Sulfoxide 1 4783 n Butyl Acetate 1 3942 Toluene 1 4969 Methyl Isobutyl Ketone 1 3957 Benzene 1 5011 Isobutyl Alcohol 1 3959 o Xylene 1 5054 2 Butanol 1 3972 Pyridine 1 5102 1 Butanol 1 3993 Chlorobenzene 1 5248 n Butyl Chloride 1 4024 p Phenethylamine 1 5332 2 Methoxyethanol 1 4021 o Dichlorobenzene 1 5514 ProStar 355 Refractive Index Detector 109 Miscibility Chart From High Purity Solvent Guide Copyright 1982 Burdick and Jackson Laboratories Inc 1953 South Harvey Street Muskegon Michigan USA 49442 Reprinted with permission of publisher Acetic Acid Acetonitrile Chloroform Cyclohexane Meth
94. tar 355 Manual Mode Prepare the mobile phase from 900 mL of HPLC grade methanol and 100 mL of distilled deionized filtered water The water and methanol should be measured separately combined and thoroughly mixed with a magnetic stirring bar and then degassed to avoid bubble formation in the RI flow cell Magnetic stirring must be continued during chromatography to avoid gravity induced phase changes NOTE Do not construct a solvent mixture by pump proportioning a combination of solvents from 2 or 3 reservoirs Refractive index detectors are too highly sensitive to small short term compositional changes in the mobile phase Never attempt to use an RI detector with gradient programming 88 2 Use a Microsorb MV C18 4 6 mm x 15 cm column part number R008620005 or equivalent reverse phase column Equilibrate column and system in the mobile phase The RI Test Sample can be purchased from Varian as a set of six sealed ampoules part number 8200504806 Use these chromatographic conditions Refer to the chromatogram in Figure 15 85 102195 00 2 OPERATION Sample RI Test Sample Mobile Phase 90 MeOH 10 H 0 at 1 0 mL min Column Microsorb MV C18 4 6 mm x 15 cm Detector Varian ProStar 355 Attenuation 8 x 10 RIU FS Polarity Normal position Refer to operating parameters Chart Speed 1 cm min Injection Volume 20 ul ProStar 355 Temperature 35 C 3 875 2 612 See 1 D 1 1
95. tar 355 reference cell Auto Zero its outputs and generate an event marker signal Reference cell purging permits the Varian ProStar 355 Refractive Index Detector to run for extended periods of time without exhibiting signal drift due to concentration changes in the reference cell medium The ProStar 355 is both reliable and sensitive in performance and straight forward and flexible in operation 85 102195 00 2 Installation Unpacking and Inspection CAUTION All phases of the installation site preparation must conform to local safety electrical and building codes These codes take precedence over any recommendations in these instructions and compliance to them is the responsibility of the customer WARNING Receiving inspection instructions are detailed in the Pre installation manual that you will have received before delivery of the detector In summary before accepting delivery you must inspect the package externally for signs of obvious damage for example crushed corners forklift punctures tears or cuts and water stains A further inspection must be made for concealed damage within the time limit stated in the terms and conditions of carriage Any shipping damage must be reported to the carrier and to your Varian Sales Office The ProStar 355 detector is packed with a number of accessory parts Do not discard the packing material until all parts are accounted for Remove the detector from the box holding the bottom of t
96. tar 800 MIB documentation 58 85 102195 00 2 Connection to a Varian Star Chromatography Workstation Figure 6 illustrates the ProStar 355 connection to the Varian Star Chromatography Workstation ProStar 355 INTEG OUT INTEG OUT Channel A Signal Cable Assembly 03 907884 01 Single D shell Channel B connector Star ADC Board Back Panel INSTALLATION J1 Analog Input Jack J2 Synchronization and Serial Communication Jack Figure 6 ProStar 355 to Varian Star Chromatography Workstation Connection to a Varian 4400 Integrator Figure 7 illustrates connection to the Varian 4400 Integrator Its input voltage is 0 1 V To monitor via recorder and integrator simultaneously you will need to order Varian part number 0200088200 Recorder Cable spade lug spade lug Attach black leads to negative terminals and clear white leads to positive terminals ProStar 355 Refractive Index Detector 59 ProStar 355 INTEG OUT INTEG OUT FG Varian 4400 Integrator Figure 7 ProStar 355 to Varian 4400 Integrator External Control of the ProStar 355 The ProStar 355 has the capability of having the following functions controlled by external devices Auto Zero purge and event marker Two items are necessary for external control of the ProStar 355 1 A separate instrument or device that is capable of generating a contact clos
97. tation avant d en d monter les panneaux de protection sous peine de s exposer a 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 24 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 ventil 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 d
98. te the performance of the ProStar 355 within the HPLC system from its performance outside the HPLC system Therefore this section begins with guidelines for testing the ProStar 355 as a stand alone Following is the Troubleshooting Table page 104 which lists the observed Problem with the Possible Cause and the Suggested Solution 102 85 102195 00 2 MAINTENANCE AND TROUBLESHOOTING Testing the ProStar 355 in Stand Alone Mode You must know how well the detector performs by itself before you can troubleshoot it in an HPLC system To perform the tests disconnect all cables from the detector except one signal cable from REC OUT to a calibrated functioning recorder The recorder should match input to the output of the Varian ProStar 355 detector Refer to page 56 for correct cabling Before proceeding verify also that the ProStar 355 shipping bolts on the optics module have been loosened see page 53 the power socket voltage matches the voltage indicated on the rear panel and the fuse is installed see page 52 and that degassed water is in the reference cell the sample cell and all hydraulic lines of the ProStar 355 Other solvents should be replaced according to the instructions in Solvent Limitations page 63 Test the performance of the ProStar 355 in stand alone mode using the Start Up Sequence function Troubleshooting a HPLC System As you go through the Troubleshooting Table you will have occasional instructions f
99. the LCD the cursor will return to the tab or cancels acommand Enter key Enter Saves an edited value in the LCD the cursor will return to the tab or confirms acommand Using the front panel controls Use the right and left arrow keys to view four main screens in the LCD display The four screens are Monitor Parameters Setting Validation Display and Span Check Monitor Screen The Monitor Screen displays refractive index temperature and status on the upper line and errors alarms and responses on the lower line The following table outlines the meaning of various codes displayed in the Monitor Screen Code Meaning LK The keys are locked ER An error has occurred RD Ready Start Up Sequence ROM ROM error RAM RAM error PARAMETER Parameter memory error HOME POSITION Null glass motion error LEAKAGE Solvent leak within flow path OPT BALANCE Exceeded null glass motion range If this error is displayed replace the solvent in the flow path If this does not fix the problem contact your local Varian representative TEMP The temperature hasn t stabilized to a constant temperature set UNSTABILIZE UNTEMP temperature 1 C over a period of 10 minutes INTENSITY The voltage of the source lamp has exceeded the limit PURGE The purge is on AUTO ZERO ZERO An Auto Zero is running S SEQ A Start Up Sequence is running F Start Up Sequ
100. tion 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 85 102195 00 2 INFORMATIONS ET MESURES DE SECURITE Precautions g n rales en matiere de s curit Les pratiques suivantes garantissent une utilisation sans risques du mat riel m Effectuer regulierement des essais d tanch it de tous les conduits d alimentation et de tous les tuyaux du syst me pneumatique m Ne pas travailler avec des conduits de gaz d form s ou perc s Installer les c
101. tituants 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 26 85 102195 00 2 INFORMATIONS ET MESURES DE SECURITE Radiations ultraviolettes Les d tecteurs CPL utilisant une source lumineuse ultraviolette comportent un cran destin a 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 a 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 Disponibilit des pieces de rechange La politique de Varian consiste fournir des pi ces de rechange pour tous les appareils et ac
102. tlet Side CAUTION Install the 5 cm long ID stainless tubing from the Accessory Kit in the OUT port of the ProStar 355 and swage the ferrule securely onto the tubing with the nut Slip the 1 5 mm ID PTFE tubing over the outside of the outlet tube Insert the opposite end of tubing into a waste bottle Use only the tubing provided for connection to the outlet Cable Connections to the ProStar 355 Recorder Connection Integrator Connection 56 Using the output signal cable supplied in the Accessory Kit connect one end to the chart recorder black lead to recorder negative terminal and red lead to recorder positive Connect the opposite end of the positive wire to the ProStar 355 REC OUT terminal Connect the negative terminal to ProStar 355 REC OUT terminal Connect the clear lead shield to the FG cable shield ground terminal NOTE The ground posts below the COM port on the rear panel see Figure 5 are not the same as the cable shield ground FG terminal Do not interchange these An output signal cable is supplied in the Accessory Kit for connecting the ProStar 355 to an integrator Connect the red lead to the INTEG OUT terminal on the rear of the ProStar 355 Connect the white lead to the INTEG OUT terminal Connect the clear lead shield to the FG cable shield ground terminal Connect the opposite end of the signal cable to the correct integrator terminals INTEG
103. treme caution to avoid spillage on skin clothing or the instrument Protective gloves are advised CAUTION Never put hydrochloric acid in the cell This acid in any concentration will corrode the cell 1 Diluted 10 20 or concentrated nitric acid is a good cleaning solution 2 The sample and reference cells should be filled with water or air blown dry before proceeding D WARNING lt A EXPLOSION HAZARD Do not allow nitric acid to contact methanol An explosion could result Completely rinse the flow cell with water following cleaning with nitric acid 94 85 102195 00 2 MAINTENANCE AND TROUBLESHOOTING 3 Connect the syringe to the IN or OUT port of the ProStar 355 To the opposite port attach plastic tubing from the cleaning solution For safety always draw the cleaning solution through the cells with the syringe Allow 3 to 10 minutes cleaning time longer cleaning periods gt 1 hour may harm the cells 4 Flush acid cleaning solutions from the cells with large amounts of water such as 1 mL min Flush for 15 to 30 minutes Other Cell Cleaning Procedures If buffers or solutions of high salt content have been in use the cells may be contaminated by precipitated salt Large amounts of distilled deionized water such as 1 mL min for up to several hours is the simplest clean up procedure An elevated cell temperature will speed dissolution The water wash can be acidified if the precipitated salt is more sol
104. trument e Does not support bacterial growth e Does not oxidize or form peroxides Examples include acetonitrile acetonitrile in water in concentrations greater than 10 V V 2 propanol xylenes and heptane NOTE Buffers must be rinsed out with water before the introduction of acetonitrile to avoid precipitation of salts 2 Turn the power off 3 Remove tubing lines to ProStar 355 and cap off Label detector with tag describing storage solvent ProStar 355 Refractive Index Detector 91 92 85 102195 00 2 Maintenance and Troubleshooting Cell Cleaning Procedure Many cases of performance degradation in sensitive instruments with flow through cells are traceable to cell contamination The use of filtered solvents with solvent reservoir filters Varian part number 2718038700 an in line filter between the pump and detector and a pre column will protect the cell from contamination and decrease the amount of cleaning required However contamination from trapped particulates or bubbles from precipitates or from thin films of residues can still occur Preparation for Cell Cleaning To introduce cleaning solution into the ProStar 355 by pump run a tubing line directly from the pump outlet to the ProStar 355 IN port bypassing the column Some materials should be injected directly into the ProStar 355 cells by syringe due to their high corrosivity or safety risk NOTE Remember that refractive index cells are stable t
105. tubing Tetrahydrofuran Because THF does oxidize you may find that if you keep solvent flowing at a reduced rate the chromatographic system takes less time to re stabilize upon start up Generally a reduced flow shutdown procedure will minimize re stabilization time the time saved is noticeable with THF as the solvent Organohalocarbons such as Methylene chloride and Chloroform Keep a small amount of flow to keep down the amount of corrosive chloride impurities in the cell 85 102195 00 2 OPERATION NOTE Ethanol stabilized chloroform does not form chloride ions readily therefore it is recommended as a mobile phase if conditions permit Continuous Power On Versus Power Off Leave the ProStar 355 power and heating on overnight and on weekends This will keep the ProStar 355 close to operating conditions and minimize stabilization time The heating temperature becomes more critical the more removed from room temperature you wish to operate Long Term Storage If the ProStar 355 will not be used for a week or more the following storage procedure should be used 1 Flush out all ProStar 355 lines reference and sample cells i e flush with Purge on then with Purge off with at least 10 mL of solvent This solvent should have the following characteristics e No dissolved salts acids bases or halides e Low vapor pressure at storage temperatures e Miscible and compatible with next probable chromatographic use of ins
106. uble in acidic solutions However do not use strongly basic pH 10 or higher solutions as these will etch the refractive index cells If contamination is suspected when a non aqueous solvent is in use flush the cells with a solvent that is 1 miscible with your mobile phase 2 a good solvent for the predicted contaminant and 3 generally of greater polarity than your mobile phase A number of HPLC references exist that classify the solvent properties of common HPLC eluents and these may be used as a guide L R Snyder Journal of Chromatography 92 223 1974 Journal of Chromatography 16 223 1978 Lamp Replacement and Adjustment Lamp Removal and Replacement NOTE Following a lamp replacement you may want to document the performance of the ProStar 355 detector for future reference The following tests are recommended e Span Adjustment page 77 e Noise and Drift Test page 81 e Chromatogram of RI Test Sample page 88 and Figure 15 ProStar 355 Refractive Index Detector 95 The light source of the ProStar 355 is a low power tungsten filament bulb As such it should have a long lifetime 10 000 hours is common Do not replace a lamp until testing indicates the lamp has failed WARNING SHOCK HAZARD Dangerous voltages exposed when cover is removed Unplug power cord Remove the ProStar 355 cover Locate the optics module Figure 16 which is a black box on the left side of the ProStar 355 The lamp is located on t
107. um von f nf 5 Jahren k nnen Ersatzteile auf der Basis solange vorhanden bezogen werden Als Ersatzteil werden hier solche elektrischen und mechanischen Einzelteile verstanden die unter normalen Bedingungen ausfallen k nnen Beispiele sind Relais Lampen Temperaturf hler Detektorelemente Motore usw Metallbleche Formteile oder Baugruppen und Gu teile PC Boards und Funktionsmodule k nnen normalerweise neuwert hnlich f r eine brauchbare Lebensdauer instandgesetzt werden und werden deshalb nur auf der Basis solange vorhanden nach dem Produktionsauslauf des Instruments geliefert werden Serviceverf gbarkeit Varian bietet seinen Kunden auch nach dem Auslaufen der Garantie eine Vielfalt von Serviceleistungen an Reparaturservice kann zu attraktiven Preisen ber eine Wartungs vereinbarung oder nach Zeit und Materialaufwand zur Verf gung gestellt werden Technische Unterst tzung und Training bieten wir Ihnen durch qualifizierte Chemiker sowohl auf einer Kontraktbasis als auch nach Ihren Erfordernissen an ProStar 355 Refractive Index Detector 43 Varian Inc 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
108. ure via a powered relay The following instruments from the Varian product line can provide this contact closure Varian SD 200 300 Pumps and ProStar 210 215 Varian SD 1 Pump Varian 9050 ProStar 310 UV Detector Varian 9002 9012 HPLC Pumps ProStar 220 230 240 e Varian 4400 Integrator with external events option and BASIC option e Varian Star 800 MIB relay control 60 85 102195 00 2 INSTALLATION 2 Acable for the contact closure signal such as e Varian part number 0200088200 spade lugs both ends e Varian part number 0200195400 3 pin Molex receptacle spade lug e Varian part number 0391972101 ProStar 355 to 9002 9012 9050 sync cable External Input Output Connections for the ProStar 355 NOTE Relays that output a TTL active low pulse will appear to the ProStar 355 as a contact closure because the ProStar 355 s events are triggered when the voltage of the positive terminal of any input is zeroed pulled low If a relay does not control events in the ProStar 355 try switching cable leads at one end CAUTION Voltages greater than TTL 0 to 5 V are not recommended as input to the ProStar 355 The closure to the ProStar 355 must be momentary i e more than 0 5 s but less than approximately 10 s A constant short across some terminals may temporarily disable some ProStar 355 features see External Control of the ProStar 35 page 60 ProStar 355 Refractive Index Detector 61 62 85 102195 00 2
109. ylene Chloride X Immiscible Dimethyl Formamide Dioxane Ethyl Ether Hexane Methanol Trimethylpentane x X Pentane Propanol 2 Tetrahydrofuran Water id ile m ane Formamide t Butyl Ether ol 2 ol c x lt e lene Chloride Ether A it Oo hy c 5 Sl S ane gt o x gt 2 imethylpentane a ethy Tetrahydrofuran Aceti Aceto Chloro Cyclo Meth Dime Dio Eth Me M Trime Penta Propal Water Methyl t Butyl Ether 110 85 102195 00 2 APPENDIX Polarity Index P From High Purity Solvent Guide Copyright 1982 Burdick and Jackson Laboratories Inc 1953 South Harvey Street Muskegon Michigan USA 49442 Reprinted with permission of publisher Listed in order of increasing polarity index Values with were estimated by L R Snyder in private communication with Burdick amp Jackson in 1979 Pentane 0 0 Isobutyl Alcohol 4 0 Trichlorotrifluoro ethane 0 0 2 Methoxyethyl Acetate 4 0 Cyclopentane 0 1 Methyl Isoamyl Ketone 4 0 Heptane 0 1 1 Propanol 4 0 Hexane 0 1 Tetrahydrofuran 4 0 Iso hexanes 0 1 Chloroform 4 1 Petroleum Ether 0 1 Methyl Isobutyl Ketone 4 2 Trimethylpentane 0 1 Ethyl Acetate 4 4 Cyclohexane 0 2 Methyl n Propyl Ketone 4 5 Hexadecane 0 5 Methyl Ethyl Ketone 4 7 n Butyl Chloride 1 0 Dioxane 4 8 Trichloroethylene 1 0 2 Et

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