Operation Manual
Contents
1. Solvent Formula Molar Mass Evaporation Boiling Point Spec Gravity Vacuum in mbar for a in g mol Energy in J g at 1013 mbar in g cm Boiling Point at 40 C Acetic acid C H O 60 0 695 118 1 049 44 Acetone C H O 58 1 553 56 0 790 556 n Amyl alcohol n Pentanol C H 0 88 1 595 37 0 814 11 Benzene C H 78 1 548 80 0 877 236 n Butanol tert Butanol C H O 74 1 620 118 0 810 25 2 Methyl 2 Propanol C H O 74 1 590 82 0 789 130 Carbon tetrachloride CCI 153 8 226 77 1 594 271 Chlorobenzene CH CI 112 6 877 132 1 106 36 Chloroform CHCI 119 4 264 62 1 483 474 Cyclohexane GA 84 0 389 81 0 779 235 Diethyl ether C H O 74 0 389 35 0 714 850 1 2 Dichlorethane C HCl 99 0 335 84 1 235 210 1 2 Dichlorethylene cis C H Cl 97 0 322 60 1 284 479 1 2 Dichlorethylene trans C H Cl 97 0 314 48 1 257 751 Diisopropyl ether C H O 102 0 318 68 0 724 375 Dioxane C H 0 88 1 406 101 1 034 107 DMF Dimethylformamide C H NO 73 4 153 0 949 11 Ethanol C H O 46 0 879 79 0 789 175 Ethyl acetate C H O 88 1 394 77 0 900 240 Heptane CH 100 2 373 98 0 684 120 Hexane CH 86 2 368 69 0 660 335 soamyl alcohol 3 Methyl 1 Butanol C H 0 88 1 595 129 0 809 14 sopropyl alcohol C H O 60 1 699 82 0 786 137 Methanol CH 0 32 0 1227 65 0 791 337 Methylene chloride Dichloromethane CH Cl 84 9 373 40 1 327 850 ethylethylketon C H O 724 473 80 0 805 243 Pentachlorethane CHCI 202 3 201 162 1 680 13 Pentane CH 724 381 36 0 626 82. B CHI Rotavapor R 220 Table of Contents Table of Contents 1 Scope of Delivery 2 6 Maintenance 23 6 1 Taking Apart the Snap Flange Coupling 23 2 Safety 3 6 2 Assembling the Snap Flange Coupling 24 6 3 Removing the Evaporating Flask Seal 24 3 Function 6 6 4 Inserting the Evaporating Flask Seal 25 3 1 Principle of Operation 6 6 5 Replacement of the Seals for the Distribution Head 25 6 6 Replacement of the Vacuum Seal 26 4 Putting into Operation 7 67 Cleaning 26 4 1 Installation Location 7 6 8 Vacuum Seal 26 4 2 Unpacking 7 6 9 Testing for Leaks 27 4 3 Setting up the Support Rod 8 6 10 Customer Service 27 4 4 Attachment of the EasyClamp 9 4 5 Removal of the EasyClamp 9 7 Taking out of Operation 28 4 6 Installation of the Reflux Glass Assembly 10 4 7 Installation of the Descending Glass Assembly 11 8 Spare Parts and Accessories 29 4 8 Installation of the Descending Glass Assembly 8 1 Glass Assemblies D D2 DB DB2 30 31 with a 2 Cooler 12 8 2 Glass Assemblies R RB C 32 33 4 9 Installation of the Receiving Fixture 13 8 3 Miscellaneous 34 4 10 Attaching and Removing Flasks 14 8 4 Accessories 37 4 11 Hose Coupling 16 4 12 Operating the Shut off tap 18 4 13 Bath Replenishment Optional 18 9 Appendix 42 4 14 Reset of the over temperature protection 19 9 1 Technical Data 42 4 15 Heating Medium 19 92 Materials Used 42 4 16 Checking Installation 19 93 Error Messages 43 9 4 FCC requirements for USA and Canada 44 5 Operation 20 95 Declaration
3. 38 B CHI Rotavapor R 220 8 Spare Parts and Accessories Fig 45 Splash Protection Component Ordering No Splash Protection Splash Protection 41201 Protective shield 41204 Protective shield seal 41259 Installation Instructions Switch the unit OFF Remove the two bolts and the plastic cover wo NR Put on the seal Plug in the plug Fasten the splash protection in place with the bolts 6 Switch the unit ON ao Operating Instructions Opening the splash protection switches the rotation OFF When the splash protection is closed again the flask starts to rotate once more when the rotation button is pressed 39 8 Spare Parts and Accessories B CHI Rotavapor R 220 Fig 46 Water valve Component Ordering No Water Valve Water valve cpl 41191 T piece 26835 Installation Instructions 1 Switch the unit OFF 2 Connect the water valve D to the water cock With optional bath replenishment 3 Z Connect the water hose to the tee and secure them with pivoting clamps S Connect the end of the water hose 5 to the control valve for bath replenishment and secure it with pivoting clamps a Connect the end of the hose at CW in on the R 220 and secure it with pivoting clamps Connect the valve plug 7 on the R 220 at the CW Valve 7 Switch the unit ON Q
4. Operating Instructions When rotation stops the cooling water and bath replenishment water switch OFF after short delay As soon as rotation starts the valve reopens and the water flows once again 40 B CHI Rotavapor R 220 8 Spare Parts and Accessories AA a Or KA Yates T H 4 vmv Bj TTC Er Banane Fura Fig 48 Connections to R 220 Component Ordering No Support for Controller Support for controller complete 41223 Installation Instructions 1 Remove the cover 2 Fasten the support using the bolt supplied with the unit Vacuum Controller V 800 for R 220 Vacuum Controller V 800 230 V 40721 Vacuum Controller V 800 120 V 40722 Vacuum Controller V 805 230 V 40723 Vacuum Controller V 805 120 V 40724 Connections Temperature probe 41076 Vacuum valve 31354 3 Control cable V 1000 38010 Control cable V 800 V 805 40758 6 Coolingwater valve 41191 41 9 Appendix B CHI Rotavapor R 220 9 Appendix 9 1 Technical Data R 220 Power Connection 4 2 kW Connection Voltage 200 VAC 230 VAC 400 VAC 10 Evaporator output Up to 4 I h water higher for other solvents depending on the heat of evaporation Frequency 50 60 Hz Site condition for indoor use only altitude up to 2000 m maximum relativ humidity 80 for temperatures up to 30 C decreasin linearly to 50 relative humidity at 40 C Am
5. B CHI Rotavapor R 220 6 Maintenance 6 4 Inserting the Evaporating Flask Seal e Insert the vapor duct e Insert the seal Using gentle pressure shove it across the lock preventing it from twisting out of position and then shove it all the way in Press it with both thumbs until it latches in position e The knob in the gearhead must come to rest in the notch in the vapour duct i a Fig 27 Inserting the evaporating flask seal 1 Fig 28 Inserting the evaporating flask seal 2 6 5 Replacement of the Seals for the Distribution Head e Open the DN70 EasyClamp by releasing the knurled nuts on all 3 bolts but do not screw the nuts completely off e Tilt the top bolt out toward the back e Open the upper and lower EasyClamp segments and carefully lift the distribution head off the glass assembly e Take out the seal A laid in at the front and replace it Fig 29 Replacement of the seals for the distribution head 25 6 Maintenance B CHI Rotavapor R 220 Fig 30 Replacement of the Vacuum Seal 1 writ Fig 31 Replacement of the Vacuum Seal 2 6 6 Replacement of the Vacuum Seal e Remove the DN70 EasyClamp completely and take off the distribution head e Pull the cylindrical seal holder out and turn it over e Insert Tool No 20075 into the metal guide on the seal and pull the seal out e Put in the new seal with the dark scraper ring facing th
6. Adjustable machine leg 41018 Clip 41110 Detent 41111 Snap flange coupling completel 41112 Protective screen 41214 36 B CHI Rotavapor R 220 8 Spare Parts and Accessories Fig 41 Lamella curtain Fig 42 Foam detector 8 4 Accessories Component Ordering No Lamella curtain Lamella curtain 41256 Individual lamella 41267 Installation Instructions 1 Put the lamella curtain on the support rod 2 Turn the lamella curtain until position is parallel to the edge of the chassis 8 Tighten the screw Foam detector The foam detection consists of a special distribution piece for the descending glass configuration the sensor power supply and the aeration valve The system will detect the rising foam and aerate the system for a split second Foam detector 40507 37 8 Spare Parts and Accessories B CHI Rotavapor R 220 El k s a Fig 43 Evaporating flask mai a ZS S c Fig 44 Drying flask Component Ordering No 6 L Evaporating flask 27470 10 L Evaporating flask 27469 20 L Evaporating flask 27468 This special flask is particularly suited for drying powdery sub stances or a homogeneous mixture of solid products The baffles attached on the circumference of the flask ensure an intensive circulation of the contents inside the flask 10 L Drying flask 28592 20 L Drying flask 28593
7. PTFE Taps Polytetrafluorethylene PTFE Table 7 Materials Used 42 B CHI Rotavapor R 220 9 Appendix 9 3 Error Messages Error messages indicate a defect on the unit and are signalled on the bath temperature display They appear with an E at the start followed by a specific number EO Message Output from the bath sensor not within the valid range Cause Sensor defective or a short circuit has occurred Action The bath heater is switched OFF The bath is lowered Rotation stops Acknowledgment Switch the unit OFF E2 Message The bath is not reaching the intended maximum height Cause The motor is defective or blocked No voltage Action The lift motor switches OFF Rotation and heating continue Acknowledgment Switch the unit OFF E3 Message The rotary drive does not reaching the required speed or is turning too quickly Cause Drive defective Mechanical blocking No power Semi conductor relay defective Action Bath heater is switched OFF Bath is lowered Acknowledgment Switch the unit OFF E4 Message Battery voltage too low Displayed only when starting the unit Cause PB battery defective Action None Acknowledgment Press the Aerate button ES Message EEPROM error Cause Hardware defect Action None Acknowledgment Press the Aerate button Work can then be continued but a Service technician must be notifi
8. gently The process is based on the evaporation and condensation of solvents in a rotating evaporating flask It is possible to work under a vacuum to ensure gentler treat ment of the product and increase productive output Distillation may be done either under a vacuum or at atmos pheric pressure A secure closeness is guaranteed in the low pressure range Fig 2 Principle of operation of the R 220 3 1 Principle of Operation Evaporation Zone The solvent in the evaporating flask is heated by the heating bath The rotation of the evaporating flask ensures an in tensive exchange of heat and mass within the contents of the flask forming a thin film of solvent on the inner surface of the flask This combination of turbulence and film prevents local overheating and ensures high distillation speed Rotary Drive The drive unit ensure the uniform rotation of the evaporating flask Cooling Zone The solvent vapor flows into the cooler at a high speed This is where the energy in the solvent vapor is transferred to the cooling medium e g water The solvent condenses Receiving Flask The receiving flask is used to collect the condensate Vacuum Cover The system pressure is reduced so as to lower the boiling point of the solvent The reduction in thermal loading that results ensures gentle treatment of the product and offers energetic advantages The pressure vacuum of distillation the temperat
9. i Seal Svi 22 Id 17 PTFE 05155 Cold trap 25124 Cold trap PLG 25978 Cold trap cover 25979 Cover seal 25981 PTFE hose Outer Diam 10 0x1 0 27277 Screwed fitting Svl 22 27289 Hose nipple 27338 Cooler Bullfrog closed PLG 27824 Shut off tap large complete 41060 Temperature sensor B complete 41076 41155 Glass holder C complete 41079 41156 pie ees Glass holder B complete 41120 EasyClamp DN25 41130 EasyClamp DN40 41131 Pivoting clamp complete 41151 Glass holder complete 41155 Clamping lever 41156 Cooler 3 coil closed PLG 41159 41241 DN40 Condensate cooler 41162 Cold trap complete 41167 Set of 10 teflon discs 41228 Set of bolts for EasyClamp DN25 41240 Set of bolts for EasyClamp DN40 41241 Inlet valve complete 41348 Connection PTFE 41354 Distribution piece R 41373 41240 DN25 Table 5 Spare parts Glass Assemblies R RB C 33 8 Spare Parts and Accessories B CHI Rotavapor R 220 8 3 Miscellaneous Component Ordering No Interchangeable receiver W Receiving flask 10L 37569 Branching piece 1 PLG 41048 Branching piece 2 PLG 41049 Outlet valve DN25 2 41061 Shut off tap small complete 41062 EasyClamp DN25 41130 Pivoting clamp complete 41151 Base for flask 41252 Ventilation cap 28582 Single receiver E Receiving flask 10L 37569 Branching piece PLG 41053 Outlet valve DN25 2 41061 Shut off tap smal
10. released and screwed off The complete seal packet can then be taken out and cleaned Wipe off the sealing lip using a soft dry cloth Clean the running surface on the vapor duct well Regular cleaning of the seal will result in a longer service life for it 6 9 Testing for Leaks After the rotary evaporator has been completely assembled and before putting it into operation i e while it is clean and dry check for tightness of the vacuum To do this evacuate the unit to below 100 mbar and then close the vacuum line The rate of pressure rise must not exceed 3 to 5 mbar per 15 minutes A greater pressure rise indicates a leak in the vacuum seal In such a case recheck all EasyClamp connections and all valves 6 10 Customer Service No intervention on or in the unit is permissible except when done by authorized Service personnel These are individuals with a well backed technical professional training and knowledge of the dangers that result from a failure to observe the safety precautions required BUCHI s Customer Service representatives have available to them a Service Manual specific to the unit in question That manual is issued only to authorized Service personnel The addresses of B CHI s official Customer Service represen tatives are shown on the back cover of this Operation Manual Please turn to these representatives should you have any malfunctions technical questions or problems in using the unit B CHI
11. scalded e Contaminated solvents that produce residues from distilla tion which could cause spontaneous reactions e g metal hydrides Solvents that can produce peroxides risk of explosions Mixtures with unknown compositions or contamination Damaged glassware Electrostatic charges while working e g during the trans fer of combustible solutions and while drying powders e Temperatures of coolants that lie below the freezing point of the distillate A clogging of the distillate cooler due to freezing out can result in too great an overpressure 2 6 Safety Precautions All regional and local laws and regulations must be observed The Rotavapor has been grounded internally to dissipate any electrostatic charges on it B CHI Rotavapor R 220 2 Safety It is always mandatory to wear personal protective gear such as protective eyewear and protective clothing The machine must never be rotated without the snap flange coupling and evaporation flask being closed No distillation may be started unless the evaporating flask is immersed in the bath There is always the risk that the neck of the flask might break off due to the great weight involved There is a risk of becoming scalded while changing evaporating flasks Wearing gloves prevents this Check the glass components regularly for possible damage spreading impact marks or cracks Never interrupt the grounding conductor protective conductor Otherwi
12. 05155 U tube PLG 27150 PTFE hose Outer Diam 10 0x1 0 27277 Screwed fitting Svl 22 27289 Cooler 3 coil PLG 27308 Hose nipple 27338 Cooler Bullfrog closed PLG 27824 Cooler Bullfrog PLG 27825 41155 U Tube Bullfrog PLG 27837 41156 41120 Bullfrog Temperature sensor B complete 41076 Glass holder B complete 41120 EasyClamp DN25 41130 EasyClamp DN40 41131 Pivoting clamp complete 41151 Glass holder complete 41155 Clamping lever 41156 41241 DN40 Cooler 3 coil closed PLG 41159 Y connection Bullfrog PLG 41166 Set of bolts for EasyClamp DN25 41240 Set of bolts for EasyClamp DN40 41241 Inlet valve complete 41348 Connection PTFE 41354 Distribution piece D PLG 41335 Table 4 Spare parts Glass Assemblies D D2 DB DB2 41240 DN25 31 8 Spare Parts and Accessories B CHI Rotavapor R 220 R RB 41159 41167 41151 KSS 41156 E 27289 41348 41060 41373 AE LA 41076 41373 41228 41162 27277 ere 41164 27289 c 25979 25981 3577 5155 25124 27338 25978 41079 41060 41348 7 A07 41373 41228 27277 41162 IT 41164 Fig 33 Spare parts Glass Assemblies R RB C 32 B CHI Rotavapor R 220 8 Spare Parts and Accessories 8 2 Spare Parts Glass Assemblies R RB C Component Ordering No Threaded sleeve Svl 22 03577
13. 50 n Propyl alcohol C H O 60 1 787 97 0 804 67 1 1 2 2 Tetrachloroethane C H Cl 167 9 247 146 1 595 35 Tetrachloroethylene C Cl 165 8 234 121 1 623 53 THF Tetrahydrofurane C H O 72 1 67 0 889 357 Toluol CH 92 2 427 111 0 867 77 1 1 1 Trichlorethane C H Cl 133 4 251 74 1 339 300 Trichlorethylene C HCI 131 3 264 87 1 464 183 Water H 0 18 0 2261 100 1 000 72 Xylol Mixture CH 106 2 389 25 o 144 0 880 M 139 0 864 p 138 0 861 Table 3 Table of Solvents CRC Handbook 65th Ed 22 B CHI Rotavapor R 220 6 Maintenance 6 Maintenance Please note all rules aimed at keeping the rotary evaporator in a functional condition These also include periodic cleaning and inspection for any damage that might have occurred Make certain that supply of power to the unit has been inter rupted before doing any maintenance work on the unit Always support the bath from below on the underside of the bath whenever doing any repair work 6 1 Taking Apart the Snap Flange Coupling e Close the two segments of the snap flange coupling e Turn the snap flange coupling by 180 until the closure faces down e Have Tool No 20075 ready at hand e Reopen the closure e Lift the 1 segment of the snap flange coupling to open it e Lift the 2 segment of the snap flange coupling to open it e With three fingers at the tip reach under the middle seg ment and raise it up e Insert Tool No 20075 in at the side between the lu
14. N45 EasyClamp connections e Insert the second cooler O together with the cooler holder into the pivoting clamp e Join the two coolers with the Y connection 9 and fix them in position with two DN45 EasyClamp connections e Align the coolers and O and the expansion vessel in their vertical positions and fix them in place with pivoting clamps 6 and e Screw the cooling water hose nipples D onto coolers and e Insert the stop cock 9 with the PTFE hose mounted on it into the distribution head and secure it with a standard joint clamp 3 e Screw the temperature sensor 4 into the support connec tion in the U tube e Check all EasyClamp connections and tighten them evenly and in parallel The installation of the receiving fixture is described on Page 18 12 B CHI Rotavapor R 220 4 Putting into Operation Fig 11 Interchangeable receiver 4 9 Installation of the Receiving Fixture All glassware used must be intact with no signs of cracks spreading impact marks or other damage Inspect the glass ware visually before installing it Single Receiver e Fasten the support ring D to the support rod with a pivoting clamp e Screw the outlet valves 3 on the receiving flask on tight using a DN25 EasyClamp connection e Place the receiving flask on the support ring With a reflux glass assembly e Bring the suppo
15. Turn the gray upper section of the grip clockwise until the shut off tap latches into the 1 position If the opening is not large enough continue turning until the shut off tap reaches the 2 position Fig 21 Bath replenishment 4 13 Bath Replenishment Optional Bath replenishment inlet Hose nipple Diam 14 mm Bath replenishment outlet Hose nipple Diam 14 mm Opening the needle valve slightly by one quarter turn pro duces a continuous supply flow Introduce the Open Shut valve supplied with the unit into the bath replenishment inlet 7 and connect it to CW Valve on the back wall of the unit This interrupts the replenishment of the bath when rotation stops The installation of the water valve is described in chapter 8 Replacement Parts Water Valve If oil is used as heating medium the bath replenishment has to be emptied and disconnected from the water inlet Otherwise there is a risk of water pouring into the hot oil bath Operating Instructions When rotation stops the cooling water and bath replenishment water switch OFF after short delay As soon as rotation starts the valve reopens and the water flows once again 18 B CHI Rotavapor R 220 4 Putting into Operation Fig 22 Reset of the over temperature protection 4 14 Reset of the over temperature protection If the heater heats up over 205 C e g if no heating medium isin the bath it is cut off b
16. ate contre les interf rences n tastes lorsque l appareil est utilis dans un environnement commercial Cet appareil g n re utilise et peut radier une nergie fr quence radio lectrique il est en outre susceprible d engendrer des interferences avec les communications radio s il n est pas install et utilis conform ment aux instructions du mode d emploi L utilisation de cet appareil dans les zones r sidentielles peut causer des interf rences n fastes auquel cas l exploitant sera amen prendre les dispositions utiles pour polier aux interf rences ses propres frais 44 B CHI Rotavapor R 220 9 Appendix 9 5 Declaration of Conformity We B CHI Labortechnik AG P O Box CH 9230 Flawil Switzerland declare on our own responsibility that the product BUCHI Rotavapor R 220 to which this declaration refers conforms to the following standards EN 61010 1 1993 IEC 1010 1 VDE 0411 1 Safety Rules for Electrical Measurement Control and Laboratory Equipment General Requirements EN 61326 1 1997 Electrical Equipment for Measurement Control and Laboratory Use EMC Requirements EN 61000 3 2 1995 1996 Limits for harmonic current emissions EN 61000 3 3 1995 Limitation of voltage fluctuations and flicker In accordance with the provisions of the EU Guidelines 73 23 EWG Guidelines for low voltage electrical equipment 89 336 EWG Electromagnetic compatibility Flawil 02 08 2005 B CHI La
17. bient temperature 5 40 C Rotary drive Induction motor with external fan 180 W Speed control Electronic continuous 5 to 140 RPM Bath output 3600 W Heat introduction 3W cm Bath dimensions Diam 480 mm x 240 mm Bath capacity 20 without flask immersed Bath pan Stainless steel X2CrNiMo 17 13 2 1 4404 or 316L Bath heater control Electronic with PT 1000 Control accuracy 2 C Range of bath temperatures 20 C 180 C Overheating protection Separate monitoring circuit Responds at 15 C over set point temperature Bath lift Linear drive Safety Class IP 65 Battery Battery PB 12V Measurement of vapor temperature PT 1000 Displays Vapor temperature bath temperature rotary soeed Aeration Integrated valve aerated in case of power failure or by button with inert gas connection Installation category degree of pollution 2 Vacuum pump Recommended suction output 2 4 m h Cooling water consumption 120 200 I h with needle valve control Cooling water pressure max 1 7 bar abs without any pulsation Weight 65 kg without glass Dimensions Refer to pertinent chapter Table 6 Technical Data 9 2 Materials Used Material Part Description Code Chassis X8CrNi 18 10 1 4301 or 304 Bath pan X2CrNiMo 17 13 2 1 4404 or 316L Glass Borosilicate 3 3 Seals Polytetrafluorethylene
18. bortechnik AG Meierseggstrasse 40 9230 Flawil Schweiz CR Le Tel 41 0 71 394 63 63 Guido Worch Fax 41 0 71 394 65 65 Qualitymanager buchi buchi com www buchi com BUCH 45 9 Appendix B CHI Rotavapor R 220 46
19. ccessories Ordering No 1 Seal tool 20057 1 Operating Manual German 96736 English 96737 French 96738 Italian 96739 Spanish 96740 Table 2 Standard Accessories B CHI Rotavapor R 220 2 Safety 2 Safety This unit has been built in accordance with the latest state of the art and with recognized rules of safety Nevertheless there are certain risks and dangers entailed with this unit e whenever the unit is operated by individuals who lack sufficient training e wheneverthe unit is used for some purpose other than its authorized use 2 1 Symbols Stop Information on dangers that can cause serious material damage and severe personal injuries or death Warning Information on dangers that can be injurious to one s health or cause material damage Note Information pointing out technical reguirements A failure to observe such information can lead to malfunctions uneco nomical operation and losses in production 2 2 Responsibilities of the Operator This unit may only be used by technical staff and by individuals who based on their training or their professional experience have a good understanding of the dangers that can arise from the its operation Staff who do not have this training and individuals who are currently in training must be given careful instructions This Operating Manual should be used as the basis for such training 2 3 Authorized Use The rotary evaporator has been de
20. ch O Lift for the bath Rotation ON OFF Rotating speed adjustment Rotating speed display 6 Heater ON OFF Input Set point temperature for bath Temperature UP DOWN Display for bath temperature Display for vapour temperature Aeration The bath is lowered automatically when the unit is switched off or in case of a power failure to ensure that the evaporating flask will in all cases remain outside the source of heat optional 5 2 Adjusting the Maximum Set Point Temperature and Automatic Lowering of the Bath in Case of a Power Interruption Setting the Maximum Set Point Temperature e Press the button SET TEMP simultaneously switching on the main breaker switch Q This activates the input for setting the maximum set point temperature e The value can be set at any level desired by pressing the DOWN and UP buttons e The input is stored and the unit switched into the operating mode only after the AERATE button is then pressed 20 B CHI Rotavapor R 220 5 Operation Adjusting the Optional Automatic Lowering of the Bath in Case of a Power Interruption e Press the button LIFT down 9 simultaneously switching on the main breaker switch This results in the display ON or OFF On The lift lowering has been switched ON Off The lift lowering has not been switched ON e To switch back and forth between ON and OFF press repeatedly on the but
21. e inside and the metal guide ring facing outward e Insert the cylinder with the seal at the back lying on the in side e Insert the seal at the front e Provisionally install the EasyClamp using 2 bolts e Set the distribution head of the glass assembly on top of the seal e Close the segments of the EasyClamp Flip the top bolt up and in and hand tighten all 3 Knurled nuts Tip When the glass assembly R is in place the vacuum seal can be taken out and or cleaned without the glass assembly having to be removed e Remove the complete DN70 EasyClamp assembly from the distribution head e Using a socket wrench release the fastening for the sup port rod e Carefully turn the glass assembly out around the support rod as an axis e Remove the seal 6 7 Cleaning Use commercially available cleaning agents to clean the glass ware Merely wipe the housing off with a damp cloth without using any organic solvents Use a commercially available de liming agent to dissolve resi dues of lime in the bath and flush the bath out well 26 B CHI Rotavapor R 220 6 Maintenance 6 8 Vacuum Seal The seal should be cleaned whenever necessary but at least once every six months During the intake phase which lasts approx 10 hours the seal will show signs of greater material loss due to wear This is normal for a PTFE seal Cleaning Before the packet of seals can be removed the distribution head must be
22. e lower condenser connection When there are two condensers D2 und DB2 the two con densers can be connected serially the additional condenser being cooled first The following is the key for all of the hose diagrams on these two pages Cooling water inlet for first condenser Cooling water outlet for first condenser Cooling water inlet for second condenser Cooling water outlet for second condenser Vacuum connection Vacuum controller T piece 026117 16 B CHI Rotavapor R 220 4 Putting into Operation Fig 18 Hose Couplings 2 The following is the key for all of the hose diagrams on these two pages Cooling water inlet for first condenser Cooling water outlet for first condenser Cooling water inlet for second condenser Cooling water outlet for second condenser Vacuum connection Vacuum controller T piece 026117 17 4 Putting into Operation B CHI Rotavapor R 220 4 12 Operating the Shut off tap The shut off tap is of a special design It does not have a continuous thread on its inside for tightening it but rather a sliding plane with two fixed latching positions The closing pres sure when it is in a closed position is provided by a prestressed spring e Insert the shut off tap on the distribution head and turn the white lower section of the grip clockwise until the shut off tap is tightly seated e To open
23. e shut off tap into the distribution head and tighten it firmly e Introduce the stop cock into the distribution head with the PTFE hose attached to it and secure it with a standard joint clamp 8 e Attach the condensate cooler to the distributor head with a DN25 EasyClamp connection and fix it in position e Screw the temperature sensor 9 into the distribution head O e Check all EasyClamp connections and tighten them evenly and in parallel The installation of the receiving fixture is described on Page 18 10 B CHI Rotavapor R 220 4 Putting into Operation Y Fig 7 Downgrade glass assembly 4 7 Installation of the Descending Glass Assembly All glassware used must be intact with no signs of cracks spreading impact marks or other damage Inspect the glass ware visually before installing it gt Fix the descending distributor head in position on the gear head using a DN70 EasyClamp connection Put the expansion vessel onto the distribution head and fix itin position with a DN45 EasyClamp connection Introduce the cooler 3 together with the cooler holder into the pivoting clamp and connect it to the distribu tion head DN45 EasyClamp connection Connect to the cooler and the expansion vessel using the U tube and fix in position with two DN45 EasyClamp connections Align the cooler 3 and the expansion v
24. ed of the problem EG Message Overload of the valve output Cause Valve defective or wrong connections Action None Acknowledgment Switch the unit OFF Table 8 Error messages To let all possible error messages appear the device must be shut off and on at least once per 24 h 43 9 Appendix B CHI Rotavapor R 220 9 4 FCC requirements for USA and Canada English This equipment has been tested and found to comply with the limits for a Class A digital device pusuant to both Part 15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communi cations These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment This equipment generates uses and can radiate radio frequency energy and if not installed and used in accordance with the instruction manual may cause harmful interference to radio communications Operation of this equipment in a residential area is like to cause harmful interference in which case the user will be required to correct the interference at his own expense Fran ais Cet appareil a t test et s est av r conforme aux limites pr vues pour les appareils num riques de classe A et la partie 15 des r glementation FCC la r glementation des radio interf rences du Canadian Depart ment of communications Ces limites sont destin es fournir une protection od qu
25. essel in their vertical positions and fix them in place with a pivoting clamp Screw the cooling water hose nipples onto the cooler Insert the stop cock 8 with the PTFE hose mounted on it into the distribution head and secure it with a standard joint clamp Fasten the vacuum connector 9 to the Y connection D with a DN45 EasyClamp connection and fix the unit in place on the lower end of the cooler with a DN45 EasyClamp Screw the temperature sensor into the support connec tion in the U tube Check all EasyClamp connections and tighten them evenly and in parallel The installation of the receiving fixture is described on Page 13 11 4 Putting into Operation B CHI Rotavapor R 220 Fig 8 Downgrade glass assembly with two coolers 4 8 Installation of the Descending Glass Assembly with a 2 Cooler All glassware used must be intact with no signs of cracks spreading impact marks or other damage Inspect the glass ware visually before installing it e Fix the descending distributor head in position on the gear head using a DN70 EasyClamp connection e Place the expansion vessel on the distribution head and fix it in position with a DN45 EasyClamp connection e Introduce the cooler together with the cooler holder into the pivoting clamp e Connect the cooler and the expansion vessel with the U tube and fix them in position with two D
26. gs on the positional lock Turn lightly until the pin becomes un latched Take the snap flange coupling assembly off h Fig 24 Snap flange coupling closed e Clean the snap flange coupling 23 6 Maintenance B CHI Rotavapor R 220 Fig 25 Assembling the snap flange coupling 6 2 Assembling the Snap Flange Coupling Insert the snap flange coupling from above until the pins in the lock latch into the hole on the lug Close the two segments of the snap flange coupling Turn the snap flange coupling again by 180 until the closure lies at the top Lift the two segments of the snap flange coupling to open them Lay the neck of the glass flask into the middle segment and raise the flask slightly Pull the segment on the left back slightly and close it until the hook latches in place Close the segment on the right Insert the closure hook and close the snap flange coupling with the closure lever A clear resistance must be felt when doing this Otherwise no seal can be fully guaranteed Fig 26 Removing the evaporating flask seal 6 3 Removing the Evaporating Flask Seal Seal the holder for the seal by 180 until the opening faces up Take hold of the seal with both hands from above and from the front and pull it out slowly Tilt the seal slightly and carefully pull it all the way out Be careful not to damage the glass centering bulge when doing so Remove the vapor duct 24
27. l complete 41062 EasyClamp DN25 41130 Pivoting clamp complete 41151 Base for flask 41252 Ventilation cap 28582 Fig 35 Single receiver E Hose Connections Softaflex hose Inside Diam 8 0 3 4 m 04113 Vacuum hose Inside Diam 10 0x5 0 3 5 m 04125 Plastic hose Inside Diam 10 0x2 0 4 5 m 27146 PTFE hose Outside Diam 10 0x1 0 2 0 m 27277 34 B CHI Rotavapor R 220 8 Spare Parts and Accessories 41094 41095 41230 41084 41229 41121 27378 Fig 36 Sealing elements Fig 37 Inlet valve complete Component Sealing elements Ordering No Support ring inlet valve 41147 Seal SVL 30 00398 Screw Cap SVL 30 03223 Screw Cap SVL 15 03549 Seal tool 20075 O ring 130x5 0 Fpm70 27378 Vapor duct 41084 Seal holder 41094 Vacuum seal 41095 Evaporating flask seal complete 41121 Easy Clamp element DN70 41135 Set of 5 O rings 64x5 0 41229 Set of 10 cover caps D11 Pa 41230 Set of distribution head sealings 41231 Glass body 41346 Inlet valve complete 41348 Connection PTFE 41354 PTFE bellow 41388 Set of 5 SVL 15 seals 41946 35 8 Spare Parts and Accessories B CHI Rotavapor R 220 Fig 38 Machine leg 41111 Fig 39 Snap flange coupling complete Fig 40 Protective screen Component Ordering No
28. nvolved Save the original packing for possible transport at a later date 4 Putting into Operation B CHI Rotavapor R 220 Fig 3 Support rod 4 3 Setting up the Support Rod Place the support rod into the holder provided for it and lower it into the foot hole at the back Fix it tight using the locking screw 0 Put the positioning ring on over the rod 150 mm below the upper edge Lay the pivoting clamp on top of the positioning ring Attach the pivoting clamp for the receiving flask 200 mm above the bottom edge of the rod When installing an interchangeable receiver Place the short support rod into the holder at the front and lower it into the foot hole Screw it tight using the locking screw Attach the pivoting clamp approx 200 mm above the lower edge of the rod B CHI Rotavapor R 220 4 Putting into Operation Fig 4 Attachment of the EasyClamp 4 4 Attachment of the EasyClamp e Carefully lay the EasyClamp around the glass and fold the top and bottom segments together closing them at their open connection point e Insert the bolt that does not have a spacer spring and tighten the knurled nuts slightly e Tighten all knurled nuts uniformly by hand Note Always tighten the Knurled nuts by hand and not to the block with the spring pressed together completely Otherwise the prestressing will be lost There must always be a gap of about 2 mm between
29. of Conformity 45 5 1 Arrangement of the Operator Control and Display Elements 20 5 2 Adjusting the Maximum Set Point Temperature and Automatic Lowering of the Bath in Case of a Power Interruption 20 5 3 Tips and Tricks 21 5 4 Table of Solvents 22 Read this Operating Manual through carefully before using the Biichi Rotavapor R 220 Always keep these Instructions readily available in the immediate vicinity of the unit so that they make be consulted at any time Chapter 2 contains important safety rules which must be ob served to ensure the safe operation of the rotary evaporator We reserve the right to make technical changes without prior notification No portion of this Operating Manual may be reproduced processed using electronic or optical systems duplicated or distributed in any form without the prior written approval of BUchi Labortechnik AG All rights reserved Buchi Labortechnik AG 1999 2001 en Version G 46 Pages R 220 Operation Manual Ordering No 96737 1 Scope of Delivery B CHI Rotavapor R 220 Fig 1 R 220 Overall View 1 Scope of Delivery Component 4 Chassis complete with control and driving unit and with heating bath 1 6L 10L or 20L Evaporation flask Receiving flask 1 x 10L Single receiver or 2 x 10L Interchangeable receivers Glass assembly Refer to Chap 4 6 4 8 for Figure Table 1 Scope of Supply Standard A
30. rt up and fix the flask in position on the dis tillate cooler using a DN25 EasyClamp connection With a descending glass assembly e Attach the branching piece to the opening at the bottom of the Y connection with a DN45 EasyClamp connection e Insert the shut off tap into the branching piece and tighten it firmly e Bring the support up and fix the receiving flask in position on the branching piece using a DN25 EasyClamp con nection Dual Receiver e Fasten the support rings to the support rods at the front and back using pivoting clamps e Screw the outlet valves firmly onto the receiving flask using DN25 EasyClamp connections e Place the receiving flasks on the support rings 0 e Screw the two shut off taps into the branching pieces and O and tighten them e Connect the branching pieces with a DN25 EasyClamp connection Place them on the receiving flasks and fasten them with DN25 EasyClamp connections With a reflux glass assembly e Bring the receiving flask up and fasten the branching piece to the condensate cooler using a DN25 EasyClamp connection With a descending glass assembly e Bring the receiving flask up and fasten the branching piece to the Y connection using a DN25 EasyClamp con nection 13 4 Putting into Operation B CHI Rotavapor R 220 4 10 Attaching and Removing Flasks Bring up the flask e With the snap flange coupling open lay the flask in po
31. s Customer Service Dept will be ready and happy to offer the following services Spare parts service Repair service Maintenance service e e e e Technical consultation 27 7 Taking out of Operation B CHI Rotavapor R 220 7 Taking out of Operation Remove all hazardous materials and clean the unit thoroughly This prevents any risk that individuals could suffer injuries due to contact with hazardous materials 7 1 Storage Always store the unit and spare parts for it in a clean and dry location 7 2 Packing Transport The original packing has been specially designed for trans porting the unit and the glass parts for it Use only the original packing materials for any further transport 7 3 Waste Disposal Table 7 in the Appendix Chapter 9 contains a list of the mate rials including their material codes used for the most important components of the unit This list has been provided in order to enable environmentally correct disposal of the rotary evapo rator It ensures that the parts can be separated and sent for appropriate recycling Please refer to the pertinent guidelines when disposing of electrical parts In addition observe all regional and local laws covering waste disposal Used batteries may be returned directly to your BUCHI re presentative for disposal 28 B CHI Rotavapor R 220 8 Spare Parts and Accessories 8 Spare Parts and Accessories Only original B CHI acce
32. se there will be the risk of an electrical shock The operator bears responsibility for providing proper instruction of his operating staff To aid him in doing this translations of this Operating Manual are also available in several other languages As an integral component of the rotary evaporator this Operating Manual must be readily available at all times to the operating staff at the location where they are using the unit The operator must inform the manufacturer immediately of any and all events relevant to safety that occur in his use of this equipment 2 7 Modifications No modifications are permissible without consulting with and obtaining the written approval of the manufacturer No glass assemblies other than those recommended by the manufacturer may be used nor may any glass components be put together arbitrarily Only those components of the rotary evaporator intended for fulfillment of its function may be installed in or removed from the unit This may be done either by hand or with the use of the tool supplied along with the unit The removal of safety devices or covers using some commercially available tool is other than for authorized commissioning personnel strictly forbidden Contact with parts that are electrically live may result in fatal injury 3 Function B CHI Rotavapor R 220 3 Function A vacuum rotary evaporator is used for guick single stage distillations that treat the product
33. signed for use in technical laboratories and in production It is authorized for use in applica tions that work with the evaporation and condensation of solvents It is used for e Evaporation of solvents and suspensions Drying of powders and granulates Re crystallization Reactions under reflux Synthesis and Cleaning of refined chemicals Recycling and concentration of solvents The authorized use of the Rotavapor also includes its care upkeep and careful handling in accordance with the provisions in this Operating Manual 2 Safety B CHI Rotavapor R 220 2 4 Unauthorized Use Any use other than those indicated above and any use that is not in conformity with the Technical Data is considered to be misuse The operator himself bears sole responsibility for all damage or injuries arising from any such use The following applications in particular are strictly forbidden e The production and processing of materials that can cause spontaneous reactions e g explosives Working without the evaporation flask being immersed in the water bath risk of breakage e The drying of hard brittle materials e g stones soil sam ples that might cause damage to the receiving flask e Sudden shock cooling of the evaporating flask The Rotavapor R 220 is not intended for work done under overpressures 2 5 Basic Dangers Basic dangers arise when working with the following e The hot water or oil bath risk of being
34. sition e Close the first segment of the snap flange coupling T h e hook must latch in e Close the second segment of the snap flange coupling e Insert the closure hook and press down the closure lever A clear resistance must be felt when this is done If not readjust the tension on the closure Adjusting the tension on the closure Open the closure hook up and turn it Turning clockwise increases pressure Turning counterclockwise reduces pressure If the flange of the evaporating flask is outside of a certain tolerance the adjustment with the hook is not possible This evaporating flask must not be used Fig 14 Adjusting the tension on the closure 14 B CHI Rotavapor R 220 4 Putting into Operation Removing flasks e Place your hand under the flask to hold it from below e Open the closure lever e Use your thumb to release the closure hook e Flip up the first segment of the snap flange coupling e With your hand under the flask lift it lightly slightly from below and relieve pressure on it e Press the hook in e Open the second segment of the snap flange coupling e Lift the flask out at the top and remove it Fig 16 Opening the second segment 15 4 Putting into Operation B CHI Rotavapor R 220 Fig 17 Hose Couplings 1 4 11 Hose Couplings In general observe the following items for all glass assemblies The cooling water inlet is always at th
35. ssories and spare parts ensure safe operation and a proper functioning of the unit The use of spare parts and accessories other than those from B CHI is permissible only with prior approval of the manufacturer The Spare Parts Catalog may be used for purposes of assembly and disassembly only in conjunction with the corresponding Chapters 4 and 7 in this Operation Manual Dis closure and distribution to third parties and manufacturing based on this manual are strictly forbidden Copyright by Buchi AG All rights reserved 29 8 Spare Parts and Accessories B CHI Rotavapor R 220 27150 27150 27289 41076 27289 41076 27308 27308 41131 ee 1165 41155 41155 41151 41156 1165 41159 1129 41335 41335 3577 5155 27338 1169 27277 41164 272771 41164 1169 41130 41130 DB DB2 27837 27837 1 r 41076 41076 41120 1165 1165 41120 27825 27824 27825 41335 41335 27277 27277 41166 41354 41354 1169 Fig 32 Spare parts Glass Assemblies D D2 DB DB2 30 B CHI Rotavapor R 220 8 Spare Parts and Accessories 8 1 Spare Parts Glass Assemblies D D2 DB DB2 Component Ordering No Vacuum connector PLG 01129 Expansion vessel PLG 01165 ii Y connection PLG 01169 Threaded sleeve Svi 22 03577 Seal Svi 22 Id 17 PTFE
36. the knurled nut and the support surface Fig 5 Removal of the EasyClamp 4 5 Removal of the EasyClamp On all EasyClamp connections only the bolt without a spacer spring has to be removed in order to open the con nection e Release the knurled nuts on all 2 or 3 bolts until the springs have been relieved Do not however screw the nut all the way off e On the bolt that does not have a spacer spring release the knurled nut far enough without removing it completely so that the bolt can be tilted out and removed as a unit e At the connection point which is now open spread the top and bottom segments apart and carefully remove the EasyClamp 4 Putting into Operation B CHI Rotavapor R 220 A O 5 6 7 Fig 6 Reflux glass assembly 4 6 Installation of the Reflux Glass Assembly All glassware used must be intact with no signs of cracks spreading impact marks or other damage Inspect the glass ware visually before installing it e Fix the reflux distribution head in position on the gear head using a DN70 EasyClamp connection e Introduce the cooler together with the cooler holder Q into the pivoting clamp and connect it to the distribu tion head DN45 EasyClamp connection e Align the cooler in a vertical position and fix it in place with the pivoting clamp e Screw the cooling water hose nipples onto the cooler O e Insert th
37. ton LIFT down e The input is stored and the unit switched into the operating mode only after the AERATE button is then pressed repeatedly 5 3 Tips and Tricks Selection of the Distillation Temperature In order to attain optimum distillation conditions the energy supplied to the distillation from the bath must be dissipated again across the cooler In order to ensure this it is best to work according to the following rule of thumb Cooling water AT2 Boilingtemperature AT1 Bath max 20 C 40 C 60 C How do you attain these conditions e Set the bath temperature at 60 C e Adjust the cooling water Its temperature should not be higher than 20 C e Allow the cooling water to flow through the cooler at a rate of about 120 150 liters hr e Select the working vacuum so that the boiling point of the solvent is at 40 C e Obtain the corresponding value for the vacuum from the Table of solvents Advantages of a Bath Temperature of 60 C e Evaporating flasks can be changed without any danger of scalding e The rate of water evaporation out of the heating bath is not yet very high e The energy inthe heating bath is being utilized very efficiently The solvent should condense out in approx 2 3 to 3 4 of the lengths of the cooling coils present 21 5 Operation B CHI Rotavapor R 220 5 4 Table of Solvents
38. ure of the heating bath the rotational speed and the size of the evapo rating flask all affect the evaporation output Refer to Chapter 5 3 for how to select the optimum conditions of distillation B CHI Rotavapor R 220 4 Putting into Operation 4 Putting into Operation The danger zone around the Rotavapor R 220 can extend outward by up to 10 m When working inside this danger zone there is a risk of damaging the glass parts which could cause them to implode The electrical connection must be installed and checked by an authorized person 4 1 Installation Location Always set the unit up on a clean stable and flat surface Never at a location where there is a great deal of personal traffic breaking or broken glass The dimensions of the rotary evaporator are Height without trolley Reflux 1700 mm Descending 1800 mm Bullfrog Reflux 1430 mm Bullfrog Descending 1550 mm with trolley Reflux 2300 mm Descending 2400 mm Width Reflux 1100 mm Descending 1250 mm Descending with 2 coolers 1250 mm Depth Single receiver 550 mm Interchangeable receivers 650 mm 4 2 Unpacking Take care not to break the glass when opening cartons that contain glassware Look for any damage after unpacking It is important that any damage in transit be identified right when unpacking If nec essary make an immediate assessment of the situation Notify the post office the railroad or the shipping company i
39. y a mechanical overtemperature protection The overtemperature protection is reset by pushing the button under the heating block 4 15 Heating Medium Never operate the heating bath when there is no heating me dium in it Suitable heating media include e Water some Borax should be added when using deionized water e Heat transfer oils suitable for use at temperatures up to 160 C e g Ucon HTF 14 Fluka AG e Water soluble polyethylene glycol e g Polyethylene glycol 600 Fluka AG After the oil bath has been standing opened for a prolonged period condensation water can collect on the bottom When the bath is used again it must be heated above 100 C with rotating flask in order to drive the water out 4 16 Checking Installation After installation has been completed and before doing the first distillation check to make sure the installation has been carried out correctly e Inspect the glass visually for possible damage e Check that all connections steam water vacuum have been fixed properly in position e Check the tightness of the vacuum 19 5 Operation B CHI Rotavapor R 220 5 Operation Make certain that the unit has been commissioned properly as described in Chapter 4 OAPI MUP 2 B GHI R tavaporA 220 MDA ee 08 Fig 23 Operator control elements for the R 220 5 1 Arrangement of the Operator Control and Display Elements Main breaker swit
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