Rotavapor® R-3
Contents
1. Switch ON OFF the instrument with the main switch To adjust the water bath temperature push the button UP and DOWN on the heating bath 68 During the adjustment the set temperature is displayed 68 Heating activity is indicated by a dot on the display NOTE As soon as the power plug is connected and the main switch is turned on the bath starts heating if the actual temperature is below the set temperature For this reason make sure that there is always water in the bath to prevent instrument damage 25 R 3 Operation Manual Version C 6 Operation 6 2 Mounting the bath guide The bath guide serves to adjust the optimal space between the Rotavapor handle and the bath Install the bath guide so that the two holes on it fit in the Rotavpor base The bath is now placed in front of the guide and the space can easily be adjusted 6 3 Mounting the evaporating flask The evaporating flask is attached to the vapor duct Take care that the vapor duct is getting no damage from accidentally contacting the flask To prefix the flask flip the metal bracket over the flask neck 8 By screwing the Combi clip clockwise the flask is connected to the vapor duct Ah NOTICE Risk of contamination and glass breakage e Clean and dry the exterior of the flask before installation and removal e Do not drop the flask e Savely support the flask at handling e Savely store the flask onto a matching flask rin2. o 10 Spare parts 032339 STJ 29 32 032341 STJ 24 40 J 2 Order number Part name Glass assembly C05 complete with 1 040640 receiving flask without seal and vapor 040627 Stop cock STJ18 8 38 duct 040641 Cold trap outer part including 23900 038000 Set of hose connections GL 14 4x bent 2x 23875 hose clips GL 14 complete straight 6x screw caps Cold trap complete including 40641 040645 23900 23875 00672 27462 003275 Clip for receiving flask S35 27479 000672 Cold trap inner trap 023875 Screw cap GL 10 027479 Cap for cold trap 023900 FPM 0 ring 3 2 7 mm 027462 Seal PTFE Viton complete 028606 Drain sleeve 037642 Set of hose connections straight GL 14 4 037287 Set of hose connections bent GL 14 4 pieces 4x olive straight with screw caps pieces 4x olive bent with screw caps 032341 Eid duct short STJ 24 40 with Combi 05593 R 3 Support rod complete Vi t short STJ 29 32 with i 032339 a Ee WEE zm 023375 Combi Clip 29 2 32 027344 Cross sleeve 027267 Combi Clip 24 40 000636 Gasket KD 22 040628 Stop cock STJ18 8 38 C 028096 PTFE hose 600mm 000646 PTFE Hose 4 7X300mm 45 R 3 Operation Manual Version C 10 3 10 4 Sealing system Product Sealing system 10 Spare parts Order number Gasket KD 22 vacuum seal 000636 Various glass parts Vapor duct Glass without Combi
3. a ak a A Ux mo ko ox pem 9 Rois ADR m ADS de and 46 10 4 Warious dlass paS i J Az a lada Be he um A E ronde Cee Rx A 46 10 5 Miscellaneous esos t a duno Gel nue de Ag dog OE Wee ci XAW eit QUN ris VO 48 11 Declaration of conformity llle 49 4 R 3 Operation Manual Version C 1 About this manual 1 About this manual This manual describes the Rotavapor R 3 and provides all information required for its safe operation and to maintain it in good working order It is addressed to laboratory personnel and operators in particular Read this manual carefully before installing and running your system and note the safety precautions in chapter 2 in particular Store the manual in the immediate vicinity of the instrument so that it can be consulted at any time No technical modifications may be made to the instrument without the prior written agreement of Buchi Unauthorized modifications may affect the system safety or result in accidents Technical data are subject to change without notice NOTE The symbols pertaining to safety WARNINGS and ATTENTIONS are explained in chapter 2 This manual is copyright Information from it may not be reproduced distributed or used for competitive purposes nor made available to third parties The manufacture of any component with the aid of this manual without prior written agreement is also prohibited The English manual is the original language version and serves as basis
4. Product Order number Floating balls 450 pieces 036405 Top cover B 491 048230 Water control valve 72 011606 Vacuum hose 16 6 017622 Cooling water hose silicone 9 6 004133 Nyflex hose 014 8 004113 Glisseal grease 60g 001330 External power supply 24 VDC 11055312 48 R 3 Operation Manual Version C 11 Declarations and requirements 11 Declaration of conformity Declaration of conformity Konfonnitatserklarung D claration de conformit Dichiarazione di conformit Declaraci n de conformidad B CHI Labortechnik AG Meierseggstrasse 40 CH 9320 Flawil 1 QD 7 C s Declares that the product Erkl rt dass das Produkt D clare par la pr sente que le produit Dichiara che il prodotto Declara que el producto Rotavapor R 3 complies with the requirements of the European Directives den Anforderungen der Richtlinien est conforme aux exigences des directives europ ennes soddisfa i requisiti delle norme europee cumple los requerimientos de las Directivas Europeas 2006 95 EEC low voltage directive 2004 108 EEC EMC directive 2006 42 EC machinery directive and is in accordance with the following standards und den folgenden Normen entspricht ainsi qu aux normes suivantes ed conforme ai seguenti standard y est conforme a los est ndares siguientes EN 61010 1 2001 Safety requirements for electrical equipment for measurement control and laboratory use Part 1 General requirements EN
5. Su 003275 9 SN N 032339 STJ 29 32 032341 STJ 24 40 List of parts Order number Part name Order number Part name 11057056 Glass assembly R 3 V complete with 1 receiving flask without seal and vapor 000646 PTFE Hose 4 7X300 mm duct Diagonal condenser R 3 V 23875 23900 Hose clips GL 14 complete Glass assembly R 3 V complete with 1 receiving flask P G Diagonal condenser R 3 V 23875 11055922 23900 Hose clips GL 14 complete 040625 PTFE drain disk PG Set of hose connections GL 14 4x bent 003275 11055921 000636 Gasket KD 22 11057057 028096 PTFE hose 600 mm 038000 2x straight 6x screw caps Clip for receiving flask S35 032341 ae duct short STJ 24 40 with Combi 040627 Stop cock STJ 18 8 38 032339 id duct short STJ 29 32 with Combi 028606 Drain sleeve Set of hose connections straight GL 14 URSUS Guri nup da USE 4 pieces 4x olive straight with screw caps 027267 Combi Clip 24 40 037287 Set of hose connections bent GL 14 4 pieces 4x olive bent with screw caps 44 R 3 Operation Manual Version C 10 2 Glass assembly C 027478 SS d 000672 TT 027462 0406287 f j gt co 7 040641 J Ll U PM aE Smee Y RE 040627 mE 027344 U Ni UL 000646 028606 Y 052891 048237 028096 023875 Sy 023900 aka Y Ta RU da a aa E d 000636 e List of parts Order number Part name
6. e Malfunction in distillation procedure Decrease the pressure manually which is not exactly defined until the distillation starts again e g sudden cooling heat flow too low etc 40 R 3 Operation Manual Version C 9 Shutdown storage transport and disposal 9 Shutdown storage transport and disposal This chapter instructs how to shut down and disposal of the instrument Information about storage and shipping conditions can also be found here 9 1 Storage and transport Switch off the instrument and remove the power cord To disassemble the Rotavapor follow the instal lation instructions in section 5 in reverse order Remove all liquids and other residues before packging the instrument NOTE It is recommended to ship the instrument and its accessories in original packaging to reduce the risk of possible transport damages A Warning Death or serious poisoning by contact or incorporation of harmful substances e Wear safety goggles e Wear safety gloves e Wear a suitable protective mask e Wear a laboratory coat e lean the instrument and all accessories thoroughly to remove possibly dangerous substances e Do not clean dusty parts with compressed air e Store the instrument and its accessories at a dry place in its original packaging A Caution Risk of minor or moderate injury by heavy weight of the instrument e Lift the instrument carefully and avoid overexertion e Do not drop the
7. 61010 2 010 2003 Safety requirements for electrical equipment for measurement control and laboratory use Part 2 010 Particular requirements for laboratory equipment for the heating of materials EN 61326 1 2006 Electrical equipment for measurement control and laboratory use EMC Requirements General requirements Fiawil July 16 2009 b tubs c Year Christian Fritsche Erich Koller Director Engineering Services Head Quality Management 49 R 3 Operation Manual Version C B CHI Labortechnik AG CH 9230 Flawil 1 Switzerland T F 41 71 39 41 71 39 63 63 65 65 www buchi com Quality in your hands
8. Cooling area The solvent vapor flows very quickly into the condenser Here the energy in the solvent vapor is trans ferred to the cooling medium mostly water so that the solvent condenses Q Receiving flask The receiving flask collects the condensed solvent Vacuum The vacuum reduces the boiling temperature and thus increases the distillation performance The evaporating performance is influenced by the distillation pressure vacuum the heating bath temperature and the rotation speed and size of the evaporating flask For information on the optimum distillation conditions see chapter Operation NOTE For information about minimum distillation conditions see section 6 Operation 16 R 3 Operation Manual Version C 4 1 1 Front side view of the Rotavapor R 3 4 Description of function Condenser Stop cock for vacuum regulation Hose to continually feed the evaporating flask with solvent Lock button to block the drive unit Knob for rotation speed of evaporating flask Receiving flask for condensed solvent Quick action jack to raise and lower the evaporating flask Q Vertical end stop Heating bath display Buttons to adjust the temperature of the heating bath O Main switch D Heating bath handle Stainless steel heating bath D Evaporating flask B Combi clip B Clamping lever for immersion angle adju
9. DANGER WARNING CAUTION and NOTICE are standardized signal words for identifying levels of hazard seriousness of risks related to personal injury and property damage All signal words which are related to personal injury are accompanied by the general safety sign For your safety it is important to read and fully understand the below table with the different signal words and their definitions Sign Signal word Definition Risk level DANGER s a a RHONE nau which if not avoided will qae result in death or serious injury 0 WARNING Maras a MUS eaten which if not avoided could EN result in death or serious injury T Indicates a h ituati hich if not avoi CAUTION uus a azardous situa lon which if not avoided may ikee result in minor or moderate injury no NOTICE Indicates possible property damage but no kxxw practices related to personal injury property damage only Supplementary safety information symbols may be placed in a rectangular panel on the left to the signal word and the supplementary text see below example Ah SIGNAL WORD supplementary Supplementary text describing the kind and level of hazard risk seriousness safety e List of measures to avoid the herein described hazard or hazardous situation information symbols n Table of supplementary safety information symbols The below reference list incorporates all safety information symbols used in this manual and their m
10. down for some minutes after use gt pb Notice Risk of instrument short circuits and damage by liquids e Do not spill liquids over the instrument or its component parts e Wipe off any liquids instantly e Ensure a safe positioning of the evaporating flask for storage e Do not move the instrument when it is loaded with liquid e Keep external vibrations away from the instrument gt Notice Risk of instrument damage by internal overpressure e Exchange clogged filters immediately e Dispose of filter immediately Notice Risk of instrument damage by wrong mains supply e External mains supply must meet the voltage given on the type plate e Check for sufficient grounding gt gt gt Notice Risk of glass breakage by exessive strains e Mount all glassware parts without strains e Check glassware for proper fixing regularly and readjust fixing points if necessary e Do not use defective glassware R 3 Operation Manual Version C 2 Safety 2 5 2 Other hazards The following warning sticker s can be found on the housing or assemblies of the Rotavapor Symbol Meaning Location Sticker label located on top of the housing and Hot item hot surface at the racks 2 5 3 Safety measures A Warning Death or serious poisoning by contact or incorporation of harmful solvents at use Before operation inspect sealings and hoses for good condition e Exchange wor
11. evaporating flask s sa kck a a kk al a al Waa ala a 34 R 3 Operation Manual Version C Table of contents 7 Maintenance and repairS llle 35 Tal CUSTOMENSEIVICS a s kon gon ORO RE RARA AA RR ERD 35 7 2 Regular service and CHECKS ba o a BA aa a 36 E21 System tighittieSS uk noce k uk Sie Ten peo AA nil uk Ah abd ae ot R 36 2 2 Housing cables and accessories x s x vow ore A a a we e 36 7 3 Sealing System and MOSES x dos a Gok e A e hae ge o dese dox Eur ape dg 36 f 9 1 Removing the vapor duct s s a a es anak ak l hom Ro 3 a Rom al 37 19 2 Oleaning the sSealsc 5 a e na dex he DR Wl a ees dae ly l due al n 37 Tos Replacing the seals weno a A ABRE RODA RR me AU RG 37 7 4 Heating Da x s s esse lk mom o RR a a Go m doy e 37 75 Glass components 4 2x A 4 4 a aha Roe AR 38 8 Troubleshooting lt s sisx kk aa kal omo UR RUE Umm ee om mom ees 39 8 1 Problem cause and corrections kK 2l 39 9 Shutdown storage transport and disposal 41 9 4 storage and transports sore aa Beha hen ya ee ee Wo RUE 2d 80W ee RR 41 9 2 Bor E Uc 42 9 3 Health and safety clearance form 2 a a 42 10 Spareparts sc 808 xw be OS ew va Ro E x E EGRE m SUR an cs na em oa 4 44 10 1 Glass assombiy V ene ia lan al A l lad a A dO o Y dd Roa 44 10 2 QGlassassembly Qs die ma wt rs RR E Ao deu RGB da ele de 45 10 9 SealingiSysterm
12. most local installation requirements Clearance at installation site e The instrument is connected to mains via a power plug The plug must be freely accessible at any time to be unplugged in case of emergency Demands on the mains circuit The mains circuit must provide the voltage that is given on the type plate of the instrument be able to handle the load of the connected instruments be equipped with adequat fusage and electrical safety measures in particular proper grounding See also technical data section 3 2 of all components regarding the different minimum system requirements NOTE e Additional electrical safety measures such as residual current breakers may be necessary to meet local laws and regulations e External connections and extension lines must be provided with an grounded conductor lead 3 pole couplings cord or plug equipment All used power cords must meet the input power requirements Notice Risk of instrument damage by wrong mains supply e External mains supply must meet the voltage given on the type plate e Check for sufficient grounding 19 R 3 Operation Manual Version C 5 Putting into operation 5 3 Assembling the Rotavapor R 3 5 3 1 Drive unit To complete the tower of the Rotavapor take the motor unit and unscrew the screw on the underside of the drive unit EA Loosen the clamping lever f
13. of the receiving flask e Rods and holders for fixing the glass assemblies e Electronic over current protection at the drive unit e Safety spring preventing the vapor duct from dropping out Glass Use of high quality inert 3 3 borosilicate glass e Use of hose connections GL 14 for preventing glass breakage Optional e The protective shield optional accessory protects operators from broken glass solvent splashes and hot heating medium in case of accidents or an implosion e With the support rod the cold trap can additionally be clamped General safety rules Responsibility of the operator The head of laboratory is responsible for training his personnel The operator shall inform the manufacturer without delay of any safety related incidents which might occur during operation of the instrument Legal regulations such as local state and federal laws applying to the instrument must be strictly followed Duty of maintenance and care The operator is responsible for ensuring that the instrument is operated in proper condition only and that maintenance service and repair jobs are performed with care and on schedule and by authorized personnel only Spare parts to be used Use only genuine consumables and genuine spare parts for maintenance to assure good system performance and reliability Any modifications to the spare parts used are only allowed with the prior written permission of the manufacturer Modif
14. regularly and replace them if necessary e g if they do not pass the vacuum sealing test described in chapter 5 5 anymore For this purpose see chapter 5 3 2 The lifetime of a seal depends on the application which where carried out with the instrument A usual lifetime is between 3 and 12 months Heating bath The inner surface of the heating bath should be cleaned if e The heating bath is calcified or contaminated e The stainless steel surface of the bath is dirty or rusty e Calcification on the steel surface appears For this purpose remove the heating bath from the Rotavapor R 3 empty it and unplug the main power supply In the case of minor calcifications use a non abrasive cleaning agent e g a bathroom cleaner or Scotch Brite If the calcification is persistent use e g acetic acid to remove it Rinse the bath thoroughly afterwards 37 R 3 Operation Manual Version C 7 Maintenance and repairs 7 5 Glass components To prolong the lifetime of the glass components consider the following Rinse glass components with water and commercial cleaning agent e g a mild soap solution NOTE We recommend cleaning all the glass components manually e Use an alkaline cleaner to remove dirt e g algae adhering within the condenser coil NOTE When a thin copper wire is introduced into the condenser coil the risk of dirt adhering to the condenser coil is reduced e Remove grease from joints After you have clea
15. until the flange is tightened to avoid that the condenser is falling down To connect the condenser with the drive unit fix it with the flange screw connection Secure the receiving flask with the clip provided for this purpose Put the stop cock in the condenser You can also secure the glass assemblies V and C using the corresponding optional support rod rod is not included and is available as an accessory 22 R 3 Operation Manual Version C 5 Putting into operation 5 3 3 Vacuum and electrical connections Connect the hose for providing the condenser with the cooling medium and 8 There is no distinction between in and out of the cooling medium For this purpose use hose connections GL 14 The used hoses must all have the same inner diameter approximately 6 mm For safety reasons secure the hoses with commercial hose pivoting clamps or cable binders Check the hoses from time to time and replace them when they are brittle Connect an adequate vacuum source to the condenser to apply the needed vacuum to the system Connect the main power cable to the heating bath Plug the connection cable from the drive unit to the 24 VDC part on the rear side of the heating bath G9 23 R 3 Operation Manual Version C 5 Putting into operation A Caution Risk of minor or moderate cuts when handling damaged glass parts e Handle glass parts with care e Visually inspect every glass p
16. Clip with Combi Clip V amp C 29 2 32 032002 032339 V amp C 032335 032341 Evaporating flasks pear shaped Content STJ 29 32 STJ 24 40 50 ml 000431 008750 100 ml 000432 008751 250 ml 000433 008754 500 ml 000434 008758 1000 ml 000435 000440 2000 ml 000436 008765 3000 ml 000437 008767 4000 ml 047991 047990 TT Drying flasks pear shaped uf oT m b Content STJ 29 32 STJ 24 40 N 500 ml 000452 011579 MV 7 1000 ml 000453 000420 Sao y 2000 ml 000454 011580 Content Distillation spider with 5 flasks Order number 50 ml with STJ 24 29 001332 100 ml with STJ 24 29 001333 46 R 3 Operation Manual Version C Reitmeyer traps agains foaming 10 Spare parts Product Order number STJ 29 32 36576 STJ 24 40 36577 Receiving flasks Content uncoated 50 ml 000421 100 ml 000422 250 ml 000423 500 ml 000424 1000 ml 000425 2000 ml 000426 Beaker flasks 1 5 version Beaker flask complete Drying flask STJ 29 2 32 034269 STJ 24 40 034770 0 5 version Beaker flask complete Drying flask STJ 29 2 32 034767 STJ 24 40 034768 Intermediate piece Content Order number Intermediate piece with valve 001006 Intermediate piece without valve 001004 Cold trap holder Product Order number Support rod complete 052893 R 3 Operation Manual Version C 10 Spare parts 10 5 Miscellaneous Miscellaneous
17. Fax or post a completed copy of this form to us in advance The declaration must arrive before the equipment Enclose a second completed copy with the product If the product is contaminated you must notify the carrier GGVE GGVS RID ADR b Inevitably the repair process will be delayed considerably if this information is missing or this procedure is not obeyed We hope for your understanding for these measures which are beyond our control and that you will assist us in expediting the repair procedure c Make sure that you know all about the substances which have been in contact with the equipment and that all questions have been answered correctly and in detail 42 R 3 Operation Manual Version C 9 Shutdown storage transport and disposal Health and Safety Clearance Declaration concerning safety potential hazards and safe disposal of waste For the safety and health of our staff laws and regulations regarding the handling of dangerous goods occupational health and safety regulations safety at work laws and regulations regarding safe disposal of waste e g chemical waste chemical residue or solvent require that this form must be duly completed and signed when equipment or defective parts were delivered to our premises Instruments or parts will not be accepted if this declaration is not present Equipment Model Part Instrument no 1 A Declaration for non dangerous goods We assure that the returned equip
18. Operation Manual Rotavapor R 3 y Ls 093244 en Table of contents Table of contents 1 About this Manual vo sa e xm e a Row a d la lb a Sa Maha nd ee a 5 Safety AN 6 2 1 USSPQUAIMCII N sergas 43 aed a a a e A 6 2 2 PIODSMUSE 3 dre e HA ma dikl d NAN IOSEPH SURE Xe IECUR va ln an ed UU UL RARA WIT k 6 2 3 Irhproper USE i ik 4 o kde al Ok OP a EUR dh dh em E es eR 6 2 4 Safety warnings and safety signals used in this manual 0 r 2 5 Product safety cw xl a E IUE RUE Y AR AAA UP RAS 9 2 5 1 Instrument related hazards s os s osoro goe e aokoe a a oaa ao a e Woe at 9 25 2 Other hazal dS m uo ac a al ra daa A ali 11 25 9 SafetymeasUIeS auo go ges A A A A 11 2 5 4 Salty elements x d Gy we o UR RUE do ad SE din edu de lA Re de eh 12 2 6 General safety rules ooa a a rss 12 3 Technicaldata o acses ox RUE e da RO A de Vala lal di raal dte Da la ka sa 13 3 1 Scope of delivery a ll rs 13 3 2 Technical data overview KK a 13 3 3 Materialsused s o soo ee Um UR al Av af AR OR OO Bom A A 14 4 Description of function kk kK kK kK 15 4 1 Functional principle of a Rotavapor R 3 0 llle 15 4 1 1 Front side view of the Rotavapor R 8 222r 17 4 1 2 Rear side view of the RotavaporR 3 a 18 5 Jnstallation e i ki a al a poo ERR RON kd a XO d akla m dk al Ja es ee aa 19 5 1 Installati n
19. Sil s t a g A Be d na k Be e te oe L 19 5 2 Electrical connections 2 al k hl lal al uk di Wa sal2 an di ak al dak lb n ak a 19 5 3 Assembling the Rotavapor B 3 e s es 20 59 Dive Un sie ropes NEK oe ce a Gp nee cep te Gosche ty AE E EREBE ERN 20 5 32 Glass palis a xo o Um ADR RRR e RR 4o Un Re RUE UR Ree Siv R ROK 21 5 3 3 Vacuum and electrical connections lt sos ss e 23 5 4 Fleatingibathimeduitis o rra whe oe eG SN E hax 24 5 5 Functional test of vacuum tightness s s sa sprr ebor d 4na ak cal dk l n aa 24 6 Operation xi a ak aya a mm al anal al m CE x RUE X ana ah a EU a nan a Qe cn aa la 25 6 1 Switching the instrument ON and OFF and setting the heating bath temperature 25 6 2 Mou ritingthebathqulde s uuo m ee gren et x enc rk Ge m K ad 26 6 3 Mounting the evaporating flask gt a a rns 26 6 4 Lowering and raising the evaporating flask gt i k ak a ee 27 6 5 Adjusting the immersion angle of the evaporating flask into the heating bath 29 6 6 Selecting the distillation conditions cns 30 6 7 DISTIN EXE he A ee a MWMIIEeIIIEEEEE E a ea i 31 6 8 Aspirating solvent directly into the evaporating flask 32 6 9 Optimizing the distillation conditions gt s kk a ka o o ka 33 6 10 When the distillation is complete K K 34 6 11 Removing the
20. art before mounting e Exchange damaged glass parts immediately e Do not touch cracks or bits of broken glass with bare hands 5 4 Heating bath medium The heating bath is suitable for the operation up to 95 C We recommend using only water as heating bath medium When the heating bath is used with water please consider the following notes Depending on the water hardness a mixture of normal water with distilled water to a ratio of 1 1 volume shares is allowed The use of the heating bath with pure distiled or deionised water is not allowed due to the corrosiveness towards stainless steel In case the use of pure deionised or distilled water as heating medium can not be avoided the addition of 1 2 g borax Na B O x 10 H O per liter water is mandatory 5 5 Functional test of vacuum tightness Carry out the functional test after all described steps for putting the instrument into operation are finished NOTE The functional test can only be carried out with a vacuum controller installed or when you have a pressure measuring device manometer connected to the hose between the vacuum source and the Rotavapor 24 R 3 Operation Manual Version C 6 Operation 6 Operation This chapter explains the operating elements and possible operating modes It gives instructions on how to operate the instrument properly and safely 6 1 Switching the instrument ON and OFF and setting the heating bath temperature
21. e 50 4000 ml up to 4000 ml Max flask content 3 kg Temperature control range room temperature 95 C Display scale scale 0 10 Set actual temperature Regulation accuracy 1 Environmental conditions for indoor use only Temperature 10 40 C Altitude up to 2000 m Humidity maximum relative humidity 80 for temperatures up to 31 C and then linearly decreasing to 50 at 40 C Bath content 4 Heating medium water distilled water we recommend to add borax in a concen tration of 0 5 g l when using deionised water Vacuum tightness of system pressure increase of 10 mbar per 3 minutes at a pressure of 100 mbar Temperature resistance protective shield lt 160 C 13 R 3 Operation Manual Version C 3 Technical data 3 3 Materials used Materials used Component Material designation Housing Rotavapor Aluminium anodized and stainless steel Housing bath and housing components PBT partially glass reinforced Bath Stainless steel Protective ring PBT partially glass reinforced Protective shield Polycarbonate Centre rotation drive Stainless steel Flange connection to cold trap Aluminum Seal NBR PTFE 14 R 3 Operation Manual Version C 4 Description of function 4 Description of function This chapter explains the basic principle of the instrument shows how it is structured and gives a functional description of the as
22. eaning General warning Electrical hazard 7 R 3 Operation Manual Version C Explosive gases explosive environment Harmful to life forms Hot item hot surface Device damage Inhalation of substances Explosive substances Fragile items content Heavy weight avoid overexertion Wear protective mask Wear laboratory coat Wear protective goggles Wear protective gloves 2 Safety R 3 Operation Manual Version C 2 Safety Additional user information Paragraphs starting with NOTE transport helpful information for working with the device or its supple mentaries NOTEs are not related to any kind of hazard or damage see example below NOTE Useful tips for the easy operation of the instrument 2 5 Product safety The Rotavapor R 3 is designed and built in accordance with current state of the art technology Nevertheless risks to users property and the environment can arise when the instrument is used carelessly or improperly The manufacturer has determined residual dangers emanating from the instrument e If the instrument is operated by insufficiently trained personnel e If the instrument is not operated according to its proper use Appropriate warnings in this manual serve to make the user alert to these residual dangers 2 5 1 Instrument related hazards Pay attention to the following safety notices A Danger Death or serious poisoning by inhalation of hazardous heating bath l
23. for all translations into other languages If you need another language version of this manual you can download available versions at www buchi com The following product names and any registered and unregistered trademarks mentioned in this manual are used for identification purposes only and remain the exclusive property of their respective owners e Rotavapor is a registered trademark of B chi Labortechnik AG 5 R 3 Operation Manual Version C 2 Safety 2 Safety This chapter highlights out the safety concept of the instrument and contains general rules of behavior and warnings from direct and indirect hazards concerning the use of the product For the users safety all safety instructions and safety messages in the individual chapters shall be strictly observed and followed Therefore the manual must always be available to all persons performing the tasks described herein 2 1 User qualification The instrument may only be used by laboratory personnel and other persons who on account of training and professional experience know of the potential dangers that can develop when operating the instrument Untrained personnel or persons who are currently being trained require careful supervision by a qualified person The present Operation Manual serves as a basis for training 2 2 Proper use The rotary evaporator has been designed for use in technical laboratories and in production It is autho rized for use in applications t
24. g or holder e Keep limbs out of crushing zone 26 R 3 Operation Manual Version C 6 Operation 6 4 Lowering and raising the evaporating flask To move the drive unit with the evaporating flask press the lift brake inside the handle GQ After unlocking the drive unit you are able to move it up and down A Caution Risk of minor or moderate burns when handling a hot heating bath e Make sure that no liquid can overflow from the bath when the evaporating flask is submerged Take care not to contact the heating bath pan while lowering the flask into the heating bath 27 R 3 Operation Manual Version C 6 Operation To limit the flask position to a fixed one lower the flask as deep as necessary into the bath by means of the quick action jack Then unscrew the position limitation at the tower of the Rotavapor and place it as high as possible Ah CAUTION e Handle glass parts with care e Do not touch cracks or bits of broken glass with bare hands 4 e Exchange damaged glass parts immediately Risk of minor or moderate cuts when handling damaged glass parts e Visually inspect every glass part for good condition before mounting 28 R 3 Operation Manual Version C 6 Operation 6 5 Adjusting the immersion angle of the evaporating flask into the heating bath If you need to operate at a different angle e g when
25. g point of the solvent is 40 C Set the rotation speed to maximum e Use the quick action jack to submerge the flask into the bath After the set vacuum has been reached wait for about 1 2 minutes to see whether distillation begins e Ifthe distillation does not start optimize the parameters decrease the pressure gradually or increase the bath temperature both possibilities lead to an increased distillation capacity see also chapter 6 9 6 8 Aspirating solvent directly into the evaporating flask Use the stop cock to fill the evaporating flask during the distillation Place the hose into the flask from where you like to fill the solvent see position in the figure above Set the Rotavapor under vacuum Open the stop cock see position in the figure above and aspirate the solvent into the evaporating flask Fill the solution you want to distill into the evaporating flask and make sure it does not exceed the filling weight of 3 kg 32 R 3 Operation Manual Version C 6 Operation 6 9 Optimizing the distillation conditions Depending on the solvent being distilled the distillation might have to be re optimized In the opti mized case the condenser should have condensation up to 2 3 to 3 4 of the condenser height If this is not the case there are two possibilities to optimize the distillation e When the heating bath has reached 60 C slowly reduce the pressure Thus the boiling point of the solvent is reduced and AT inc
26. hat work with the evaporation and condensation of solvents e Evaporation of solvents and suspensions e Synthesis and cleaning of refined chemicals e Recycling and concentration of solvents e Re crystallization e Drying of powders and granulates 2 3 Improper use Applications not mentioned in section 2 2 are considered to be improper Applications which do not comply with the technical data see section 3 of this manual are also considered to be improper The operator bears the sole risk for any damages or hazards caused by improper use The following Uses are expressly forbidden e Use of the instrument in explosive environments e Use of the instrument to process substances that are used as food feed cosmetic or pharmaceu tical afterwards e The production and processing of materials that can cause spontaneous reactions e g explosives metal hydrids or solvents that can form peroxides Processing with explosive gas mixtures e Processing with oil Working without the evaporating flask being immersed in the heating bath risk of breakage e The drying of hard brittle materials e g stones soil samples that might cause damage to the receiving flask e Sudden shock cooling of the evaporating flask and other glass parts e Installation or use of the instrument in rooms which require ex protected instruments 6 R 3 Operation Manual Version C 2 Safety 2 4 Safety warnings and safety signals used in this manual
27. he malfunc tion occurs again contact the Buchi customer service Bath does not heat e Mains switch off e Instrument is not connected to power supply e Over temperature protection was activated e Fuse defective Switch on mains switch Check mains connection Let the bath cool down and empty it Then push the tempera ture sensor reset button at the bottom side of the heating bath e g by means of a tooth stick see picture below Replace the fuse If the malfunction occurs again contact the Buchi customer service System is leaking e Joints have not been greased e Hose connections have not been fixed correctly or are defective e Hoses are leaky brittle e Sealing system has been installed Grease joints Check hose connections Replace hoses Check sealing system incorrectly e Seal is defective e Replace seal Vacuum is not reached e Reduce evaporation at Rotavapor e Empty receiving flask e Water pressure of water jet pump is too low Open water tap completely Distillation not optimized Manually decrease the pressure until the distillation starts again 39 R 3 Operation Manual Version C 8 Troubleshooting Malfunctions and their remedy cont Malfunction Possible cause Corrective measure Distillation stopped e Back evaporation from the receiving Empty receiving flask and restart although not dried out flask is too strong distillation completely especially for solvent mixtures
28. i customer service offices are given on the Buchi website under www buchi com If malfunctions occur on your instrument or you have technical questions or applica tion problems contact one of these offices The customer service offers the following e Spare part delivery e Repairs e Technical advice 35 R 3 Operation Manual Version C 7 Maintenance and repairs 7 2 Regular service and checks To maintain the system in good working order the checks described in this section should be performed regularly Defective or worn out parts must be exchanged directly to ensure safe use and optimal efficiency 7 2 1 System tightness To evaluate the system tightness evacuate the unit to below 100 mbar and then close the vacuum line The rate of pressure rise must not exceed 30 mbar per 10 minutes A greater pressure rise indicates a leakage In such a case recheck all connections sealing rings and valves for proper seating 7 2 2 Housing cables and accessories Check the housing cables and accessories for visible defects cracks kinks etc Clean housing parts regularly with a damp cloth Soapy water can be used as cleaning agent All housing parts must be completely dried before the system can be connected to mains again A WARNING Death or serious burns by electric current at cleaning e Switch off the instrument e Disconnect the power cord and prevent unintentional restart A e Wait until the instrument is comple
29. ications Modifications to the instrument are only permitted after prior consultation and with the written approval of the manufacturer Modifications and upgrades shall only be carried out by an authorized Buchi technical engineer The manufacturer will decline any claim resulting from unauthorized modifications 12 R 3 Operation Manual Version C Technical data 3 Technical data This chapter introduces the reader to the instrument specifications It contains the scope of delivery technical data requirements and performance data Scope of delivery Check the scope of delivery according to the order number NOTE For detailed information on the listed products see www buchi com or contact your local dealer Technical data overview Technical data Rotavapor R 3 R 3 Heating bath Glass assemblies VC Dimensions W x H x D 430 x 535 x 315 mm 285 x 240 x 330 mm Weight 13 14 kg depending on the glass 4kg assembly Connection voltage 24 VDC 100 120 V or 220 240 V 10 Fusage T 12 5 AL 250V 100 120 V version T 6 3 AL 250V 220 240 V version Mains connection via connection to heating bath R 3 or external power supply available on request 3 pole P N E via power cord Frequency 50 60 Hz Power consumption 30W 1700 W Installation category Il Il Degree of protection IP21 IP21 Pollution degree 2 2 Rotation speed range 20 280 rpm Flask siz
30. instrument or its transport box e Place the instrument on a stable even and vibration free surface e Keep limbs out of crushing zone 41 R 3 Operation Manual Version C 9 Shutdown storage transport and disposal 9 2 Disposal To dispose of the instrument in an environmentally friendly manner a list of materials is given in chapter 3 This helps to ensure that the components are separated and recycled correctly Make especially sure to dispose of the gas springs appropriately Please follow valid regional and local laws concerning disposal NOTE When you send the instrument back to the manufacturer for repair work please copy the health and safety clearance form on the following page fill it in and enclose it in the instrument package 9 3 Health and safety clearance form Declaration concerning safety potential hazards and safe disposal of waste e g used oil Safety and health of our staff laws and regulations regarding the handling of dangerous goods occupational health and safety regulations safety at work laws and regulations regarding safe disposal of waste e g waste oil require that for all Rotavapors and other products this form must be send to our office duly completed and signed before any equipment is repaired or dispatched or to our prem ises Products will not be accepted for any procedure and handling and repair DKD calibration will not start before we have received this declaration 8
31. iquids e Do not inhale fumes from the heating bath e Keep the heating bath temperature on a low level e Obtain the material safety data sheets of all used liquids e Wear appropriate personal protective equipment e Do not use liquids of unknown composition e Directly withdraw released fumes and gaseous substances by sufficient ventilation Only operate the instrument in ventilated environments A Warning Death or serious injuries by formation of explosive atmospheres inside the instrument Directly withdraw released fumes and gaseous substances by sufficient ventilation at filling e Before operation check all gas connections for correct installation e Establish inert system atmosphere before processing substances that can form explosive or reactive gases or powders e Check for proper earth connection to lead off electrostatic charges PPP A Warning Death or serious injuries by use in explosive environments e Do not operate the instrument in explosive environments e Do not operate the instrument with explosive gas mixtures e Before operation check all gas connections for correct installation e Directly withdraw released gases and gaseous substances by sufficient ventilation p 9 R 3 Operation Manual Version C 2 Safety A Caution Risk of minor or moderate burns when handling hot parts e Do not touch hot parts or surfaces e Let the evaporating flask cool
32. ment has not been used in the laboratory and is new was not in contact with toxic corrosive biologically active explosive radioactive or other dangerous matters L is free of contamination The solvents or residues of pumped media have been BUCHI drained E 1 B Declaration for dangerous goods List of dangerous substances in contact with the equipment Chemical substance Danger classification We assure for the returned equipment that all substances toxic corrosive biologically active explosive radioactive or dangerous in any way which have pumped or been in contact with the equipment are listed above C the equipment has been cleaned decontaminated sterilized inside and outside and all inlet and outlet ports of the equipment have been sealed 2 Final Declaration We hereby declare that we know all about the substances which have been in contact with the equipment and all questions have been answered correctly we have taken all measures to prevent any potential risks with the delivered equipment Company name or stamp Place date Name print job title print Signature Health and Safety Clearance 20081110 doc 20081110 Version 1 0 Page 1 1 43 R 3 Operation Manual Version C 10 Spare parts Spare parts Glass assembly V y 11055921 040627 A 11055922 P G N 028606 B sas Y 000636 048237 000646 0238 023900 028096 m
33. n out or defective parts immediately e Before operation check the instrument for correct assembling and proper sealing e Only operate the instrument in ventilated environments Directly withdraw released gases and gaseous substances by sufficient ventilation e Wear safety goggles e Wear safety gloves e Wear a suitable protective mask e Wear a laboratory coat 11 R 3 Operation Manual Version C 2 5 4 2 6 2 Safety Safety elements Electronics The heating bath is equipped with a mechanical over temperature protection The mechanical over temperature protection consists of a bimetal thermostat that in case of over temperature over 145 C directly interrupts the power supply It has to be set back manually after the bath has cooled down see also chapter 8 The electronic over temperature protection controls the temperature limit actual bath temperature may not exceed the given temperature by 2 C for more than 2 minutes the heating rate actual temperature may not rise by more than 5 C during 5 seconds and the function of the temperature sensor e The heating bath is equipped with safety fuses e The heating bath is equipped with a thermostatic control of the bath temperature to prevent the product from overheating Parts in direct contact with the instrument e Combi clips for fixing the evaporating flask and for safe removal of fixed ground glass joints Ball joint clip for safe fixing
34. ned and completely dried each glass component visually inspect the components for glass splinters or cracks Since these components are under vacuum when the Rotavapor R 3 is operating they are subject to strain Regularly check the glass components for damages and only use glassware that is in perfect condition Glassware with cracks stars or other damages can break during operation 38 R 3 Operation Manual Version C 8 Troubleshooting 8 Troubleshooting This chapter helps to resume operation after a minor problem has occurred with the instrument It lists possible occurrences their probable cause and suggests how to remedy the problem The trouble shooting table below lists possible malfunctions and errors of the instrument The operator is enabled to correct some of those problems or errors by him herself For this appropriate corrective measures are listed in the column Corrective measure The elimination of more complicated malfunctions or errors is usually performed by a Buchi technical engineer who has access to the official service manuals In this case please refer to your local Buchi customer service agent 8 1 Problem cause and corrections Malfunctions and their remedy Malfunction Possible cause Corrective measure Instrument does not work e Mains switch off e Instrument is not connected to power supply e Fuse defective Switch on mains switch Check if mains connection is okay Replace the fuse If t
35. o keep the instru ment in a good and safe working condition All maintenance and repair work requiring the opening or removal of the instrument housing must be carried out by trained personnel and only with the tools provided for this purpose NOTE Use only genuine consumables and spare parts for any maintenance and repair work in order to assure warranty and continued system performance Any modifications of the Rotavapor R 3 or parts of it need prior written permission of the manufacturer A CAUTION Risk of minor or moderate cuts when handling damaged glass parts e Handle glass parts with care e Visually inspect every glass part for good condition before mounting e Exchange damaged glass parts immediately e Do not touch cracks or bits of broken glass with bare hands Notice Risk of instrument damage by liquids and detergents e Empty the heating bath and all glass accessories prior to maintenance and repair action e Do not spill liquids over the instrument or parts of it e Wipe off any liquids instantly e For the housing use ethanol or sopy water as detergent only Pp 7 1 Customer service Only authorized service personnel are allowed to perform repair work on the instrument Authoriza tion requires a comprehensive technical training and knowledge of possible dangers which might arise when working at the instrument Such training and knowledge can only be provided by Buchi Addresses of official Buch
36. operating with a small flask the angle can be changed as follows e Do not change the immersion angle while the instrument is operating A e Always support the glass assembly with one hand when loosening the anchoring Turn off the instrument Stabilize the glass assembly with one hand and loosen the screw on the underside of the drive unit Set the condenser in the desired position by tilting the drive unit accordingly Retighten the screw on the underside of the drive unit Notice Risk of glass breakage 29 R 3 Operation Manual Version C 6 Operation 6 6 Selecting the distillation conditions To achieve optimal distillation conditions the distillation energy supplied by the heating bath must be removed by the condenser To ensure this operate the instrument according to the following rule of thumb Cooling water max 20 C Vapor 40 C Bath 60 How are these conditions achieved e Set the bath temperature to 60 C e Set the cooling water temperature not higher than 20 C e Allow cooling water to flow through the condenser at approximately 40 50 l h e Define the operating vacuum in such a way that the boiling point of the solvent is 40 C Advantages associated with bath temperatures of 60 C e The evaporating flask can be replaced without risk of burns e The evaporation rate of the water from the heating bath is low low energy loss e The heating bath energy is
37. or immersion angel adjustment 69 Place the drive unit on the axis of the tower The angle limiter on the axis must be placed in the cavity of the rear cover of the drive unit completely EN The motor must be placed within a space of approx 4 5 mm space between motor unit and tower Fix the motor with the thumb screw on the bottom side of the motor Make sure that the motor can not be removed from the tower 20 R 3 Operation Manual Version C 5 Putting into operation Finalize the mounting of the motor by tightening the clamping lever on the drive unit Place the Rotavapor on the laboratory table and add the heating bath in front of the tower A Caution Risk of minor or moderate injury by wrong assembly e Screw in the fixing thumb screw completely e Tighten the angle fixing leverage 5 3 2 Glass parts Mount the sealing on the flange of the condenser Q9 ZEN AA b Take the vapor duct and put it trough the motor unit This should give a click when it is mounted prop erly and be tight on the Rotavapor Place the condenser together with the seal in the flange of the drive unit Take care that the seal is placed around the vapor duct without damaging the PTFE part 21 R 3 Operation Manual Version C 5 Putting into operation Hold the condenser with your left hand
38. reases resulting in an increase of distillation capacity e When the heating bath has reached 60 C increase the bath temperature Thus AT increases resulting in an increase of distillation capacity as well 3 4 NOTE When the bath temperature is increased not all of the additional energy is used for distillation but a major part is discharged into the environment due to the increasing difference between the heating bath and the ambient temperature 33 R 3 Operation Manual Version C 6 Operation 6 10 When the distillation is complete When the distillation is complete replace the receiving flask to eliminate the risk of back evaporation Then continue distillation Repeat this process until all desired solvent is distilled off At the end of the distillation stop the rotation pull the flask off and aerate the system If you do not intend to immediately perform another distillation turn off the heating bath and cooling water supply to save energy and resources 6 11 Removing the evaporating flask Turn the Combi clip counterclockwise 69 while supporting the flask with the other hand Remove the metal bracket from the flask and release the flask see postion and 9 34 R 3 Operation Manual Version C 7 Maintenance and repairs 7 Maintenance and repairs This chapter gives instructions on maintenance work to be performed in order t
39. semblies 4 1 Functional principle of a Rotavapor R 3 With a Rotavapor single step distillations are performed quickly and in a product friendly manner The basis of this procedure is the evaporation and condensation of solvents using a rotating evaporator flask under vacuum Distilling products under vacuum increases the performance and helps to protect the products Standard vacuum applications Due to its sophisticated sealing system a highly stable vacuum level can be reached in combination with a vacuum controller and a vacuum pump The vacuum also eliminates unwanted or hazardous emissions of vapors during the process and serves as an important safety feature The low pressure decreases the boiling point of the medium inside the Rotavapor This allows to treat the product gently at even higher evaporation performance compared to environmental pressure operation 15 R 3 Operation Manual Version C 4 Description of function Evaporation area The solvent is heated by means of a heating bath At liquids the turbulent mixing inside the rotating evaporating flask results in an increased evaporation rate The rotation also prevents a local overheating of the mixture and bumping Rotation drive including vapor duct The drive unit ensures that the evaporating flask rotates evenly The integrated vapor duct transports the vapor from the evaporation area to the cooling area 68
40. stment 17 R 3 Operation Manual Version C 4 Description of function 4 1 2 Rear side view of the Rotavapor R 3 O Evaporating flask Q Connection cable between heating bath and drive unit Q Water bath O Replenishment hose Fuse Cooling water connection of condenser Power supply for heating bath Cooling water connection of condenser Q Power supply for the drive unit of the R 3 Vacuum connections to condenser 24 VDC 18 R 3 Operation Manual Version C 5 Putting into operation 5 Installation This chapter describes how the instrument is installed and gives instructions on initial startup NOTE Inspect the instrument for damages during unpacking If necessary prepare a status report imme diately to inform the postal company railway company or transportation company Keep the original packaging for future transportation 5 1 Installation site Place the instrument on a stable horizontal plane and consider the maximum product dimensions Perform the distillations under vacuum with the Rotavapor R 3 placed inside a fume hood If this is not possible due to shortage of space mount the protective shield optional accessory and lead the exhaust gas from the pump into the fume hood 5 2 Electrical connections The Rotavapor is aimed to be installed mobile It is available with multiple kinds of power plugs to meet
41. tely dry before reconneting to mains 7 3 Sealing system and hoses Check for wear and clean the vacuum seal at least every six month Check all other sealings and hoses for wear at least yearly Visually examine the hose connections regularly When hoses become cracked and brittle replace them with new ones Grease the stop cock joint regularly to achieve optimum tightness of the system Exchange sealings with scratches or other harms directly NOTE e To prevent damaging the seals never apply grease or touch them with sharp objects e PTFE sealings need a 10 hours run in period to reach their optimum tightness condition This is normal for a PTFE seal 36 R 3 Operation Manual Version C 7 3 1 7 3 2 7 3 3 7 4 7 Maintenance and repairs Removing the vapor duct To remove the vapor duct proceed as follows e Switch off the instrument e Hemove the evaporating flask from the instrument e Press the button on the front of the drive unit see postion e Turn the Combi clip clockwise until the vapor duct is released see postions and 9 Cleaning the seals To prolong the lifetime of the seals rinse them regularly with water especially if bumping occurred during the distillation or if working with crystalline products Afterwards dry them with a soft cloth To remove the seals see chapter 5 3 2 Replacing the seals Seals are subject to wear and tear thus you should check them
42. used at a good degree of efficiency This rule can also be applied to lower bath temperatures e g Cooling water 0 C Vapor 20 Bath 40 C 30 R 3 Operation Manual Version C 6 Operation 6 7 Distilling To start operating the instrument the following conditions have to be fulfilled e All electrical connections are established correctly e All sealing are inserted correctly e Alljoints are greased To start operating the instrument proceed as follows e Switch on the instrument e Allow cooling water with a temperature not higher than 20 C to flow through the condenser at approx 40 50 l h e Set the heating bath temperature to the desired value as described above and wait until the heating medium has reached its operating temperature e Fill the solution you want to distillate into the evaporating flask and make sure it does not exceed the filling weight of 3 kg e Mount the evaporating flask see chapter 6 3 e To adjust the rotation speed of the evaporating flask turn the knob on the front side of the drive unit The rotation speed can be adjusted between 20 to 280 rpm 31 R 3 Operation Manual Version C 6 Operation e To apply the needed vacuum to the instrument switch on the external vacuum source or open the corresponding isolating valve The vacuum can be adjusted while closing or opening the stop cock at the condenser 8 NOTE e Choose the pressure in such a way that the boilin
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