1593663 en Rotavapor® R100 Operation Manual
Imprint Product Identification: Operation Manual (Original) Rotavapor® R100 11593663 en Publication date: 12.2014, Version B BÜCHI Labortechnik AG Meierseggstrasse 40 Postfach CH9230 Flawil 1 EMail: quality@buchi.com BUCHI reserves the right to make changes to the manual as deemed necessary in the light of experi ence; especially in respect to structure, illustrations and technical detail. This manual is copyrighted.
BÜCHI Labortechnik AG Contents Contents 1 About this document........................................................................................................... 5 1.1 1.2 1.3 1.4 Warning notices in this document........................................................................................................ Symbols ............................................................................................................................................... 1.2.1 Warning symbols ........
Contents BÜCHI Labortechnik AG 5 Installation.......................................................................................................................... 21 5.1 5.2 5.3 5.4 5.5 5.6 5.7 5.8 5.9 Installation site ................................................................................................................................... Mounting the rotary drive unit ............................................................................................................
BÜCHI Labortechnik AG 1 About this document | 1 About this document These operating instructions describe the Rotavapor® R100 at the time supplied. They are an integral part of the product and contain important information that is nec essary for safe operation and maintenance. These operating instructions apply to all variants of the Rotavapor® R100 and are in tended primarily for laboratory staff.
1 | About this document BÜCHI Labortechnik AG Symbol 1.2.2 Symbol Meaning Hot surface Healthharming or irritant substances Risk of hand injury Strong magnetism Mandatory directive symbols Symbol 1.2.3 Meaning Meaning Symbol Meaning Wear safety goggles Wear protective clothing Wear protective gloves Heavy load, do not lift without assistance Other symbols NOTE This symbol draws attention to useful and important information.
BÜCHI Labortechnik AG Safety | 2 2 Safety 2.1 Intended use The Rotavapor® R100 is intended for evaporating and condensing solvents. It can be used in laboratories and production facilities for the following operations: Evaporating and condensing solvents and suspensions Synthesis and purification of refined chemicals Recycling and concentration of solvents Recrystallization Drying of powders and granulates 2.
2 | Safety BÜCHI Labortechnik AG 2.3 Staff qualification Unqualified persons are unable to identify risks and are therefore exposed to greater dangers. The device may only be operated by suitably qualified laboratory staff. These operating instructions are aimed at the following target groups: Users Users are persons that meet the following criteria: They have been instructed in the use of the device.
BÜCHI Labortechnik AG 2.4.2 Safety | 2 High internal pressure The evaporation of fluids can produce high pressures inside the flask or the con denser. If that pressure becomes too great, the glass components could explode. u Make sure that the internal pressure inside the glass components is never greater than atmospheric pressure. u When distilling without a vacuum, set the vacuum pump to atmospheric pressure so that excess pressure is automatically dissipated.
2 | Safety BÜCHI Labortechnik AG u Always wear appropriate personal protective equipment such as safety goggles, protective clothing and gloves. u Make sure that the personal protective equipment meets the requirements of the safety data sheets for all chemicals used. 2.6 Modifications Unauthorized modifications may impair safety and lead to accidents. u Use only genuine BUCHI accessories, spare parts and consumables.
BÜCHI Labortechnik AG Product description | 3 3 Product description 3.1 Description of function The Rotavapor® R100 is a rotary evaporator with the aid of which singlestage distil lation can be carried out quickly without unduly stressing the product. The basis of the process is the evaporation and condensing of solvents using a rotating evaporating flask under vacuum. Distillation under vacuum increases capacity and is more gentle on the product.
3 | Product description BÜCHI Labortechnik AG 3.2 Configuration 3.2.1 Front view 13 Fig. 1: Configuration of R100 with Vcondenser 1 Condenser 9 Rotary drive unit 2 Glass stopcock 10 Combiclip 3 Solvent feeding 11 Evaporating flask 4 Power supply for rotary drive unit 12 Heating bath 5 Receiving flask 13 Master switch 6 Handle for height adjustment 7 Lower vertical stop 8 Vertical operating range adjuster Fig.
BÜCHI Labortechnik AG 3.2.2 Product description | 3 Rear view Fig. 3: Rear view R100 1 Power supply connection 3 Vacuum connection 2 Fuse 4 Coolant fluid connection 5 Power supply for rotary drive unit 3.2.3 Heating bath user interface 4 Fig.
3 | Product description 3.2.4 BÜCHI Labortechnik AG Typical application In order to use the Rotavapor® R100 to best effect, we recommend that it is used to gether with the following peripheral devices: Recirculating Chiller F-100 Fig. 5: Rotavapor® R100 system 1 Recirculating Chiller F100/F105 2 Rotavapor® R100 3 Vacuum Pump V100 with Interface I100 The Vacuum Pump V100 is designed for evacuating laboratory apparatus with the aid of a PTFE membrane.
BÜCHI Labortechnik AG 3.2.5 Product description | 3 Type plate The type plate is on the righthand side of the Rotavapor® R100. BUCHI Operations India Pvt Ltd 394230 Surat / India Type: R-100 SN: 1000000000 Volt: 100 – 240 VAC Frequ.: 50/60 Hz Power: 210 W Built: 2014 Designed by BUCHI in Switzerland, Made in India 1 2 3 4 5 6 7 8 9 11 10 Fig.
3 | Product description BÜCHI Labortechnik AG 3.2.6 Warning symbols on the device The device carries the following warning symbol: 3.
BÜCHI Labortechnik AG Product description | 3 3.4 Technical data 3.4.1 Rotavapor® R100 3.4.2 Dimensions (W x H x D) 617 x 898 x 502 mm (inc. condenser and heating bath) 480 x 626 x 502 mm (w/o condenser and heating bath) Weight 18 – 19 kg (depending on glassware included) Voltage 24 V DC Power consumption 30 W Enclosure rating IP21 Immersion angle 0 – 35° Adjustable height 150 mm (+ 100 mm optional extension) Rotation speed 20 – 280 rpm Flask size 50 – 4000 mL Max.
3 | Product description 3.4.3 BÜCHI Labortechnik AG Ambient conditions Max. altitude above sea level 2000 m Ambient temperature 10 – 40 °C Maximum relative humidity 80 % for temperatures up to 31 °C decreasing linearly to 50 % at 40 °C The Rotavapor® may only be used in indoor areas. 3.4.4 18/60 Materials Component Material Rotavapor housing Anodized aluminium with powder coating Heating bath housing PBT, partially glassfiber reinforced Heating bath Stainless steel 1.
BÜCHI Labortechnik AG Product description | 3 3.5 Safety features 3.5.1 Overheat cutout To protect against overheating, the heating bath has a thermostatic bath temperature control. In addition it is fitted with an electronic and a mechanical overheat cutout.
4 | Transport and storage BÜCHI Labortechnik AG 4 Transport and storage 4.1 Transport IMPORTANT Risk of breakage due to incorrect transportation u Make sure that the device is fully dismantled and all parts of the device are safely packed in such a way as to prevent breakage, ideally in the original box. u Avoid sharp movements during transit. u After transportation, check the device and all glass components for damage. u Damage that has occurred in transit should be reported to the carrier.
BÜCHI Labortechnik AG Installation | 5 5 Installation 5.1 Installation site The installation site must meet the following requirements: Firm and level surface Space requirements: at least 620 mm x 510 mm (W x D) If distilling under vacuum, there must be a fume hood available. Wherever possible, the Rotavapor® R100 should be set up inside the fume hood.
5 | Installation BÜCHI Labortechnik AG 5.3 Fitting the vapor duct and condenser 1 2 2 3 4 u Insert vapor duct (4) into the rotary drive unit. The vapor duct snaps into place with an audible click. u NOTICE! Risk of seal damage if fitted incorrectly. Insert seal (2) into the flange of the condenser (1) as shown. u Fit condenser (1) into the rotary drive unit, keeping it straight as you do so.
BÜCHI Labortechnik AG 5.4 Installation | 5 Fitting the glass stopcock Materials required: Grease Glisseal 40 blue (order number 048197) u Connect a supply tubing for solvent (2). u Apply a thin coat of Grease Glisseal 40 blue to the glass stopcock (1). u Insert glass stopcock into the condenser and turn to the desired position. The glass stopcock performs various functions depending on its position: Glass stopcock handle pointing forwards or backwards: the system is sealed.
5 | Installation BÜCHI Labortechnik AG 5.5 Connecting the vacuum and cooling media tubing To achieve optimum distillation, all devices in the system should be matched to one another. Therefore, we recommend that the Rotavapor® R100 is used together with the BUCHI Vacuum Pump V100 and the BUCHI Recirculating Chiller F100 or F105 (see Chapter 3.2.4 "Typical application", page 14). u Connect cooling media tubes to the two coolant connections (2) and (3) using GL14 cap nuts.
BÜCHI Labortechnik AG 5.6 Installation | 5 Electrical connections u Make sure that the available power supply matches the rating indicated on the type plate. u Plug the rotary drive unit connecting lead into the socket (2) on the heating bath. u Plug the power cord into the socket (1) on the heating bath and then into a mains power socket. u If an extension lead is required, make sure that it is earthed and has a suitable power rating. 5.
5 | Installation BÜCHI Labortechnik AG 5.8 Setting up and filling the heating bath 1 2 u Locate the heating bath (1) in the Lshaped cutout in the Rotavapor base (2). IMPORTANT Risk of heating bath corrosion due to use of unsuitable heating fluid u Do not use pure distilled water or deionised water. u If pure distilled or deionised water has to be used, add 1 to 2 g of Borax (Na2B4O7 x 10 H2O) per litre of water. The recommended fluid for use in the heating bath is water.
BÜCHI Labortechnik AG Operation | 6 6 Operation 6.1 Preparations 6.1.1 Preparing the heating bath CAUTION Risk of skin burns from hot fluids and surfaces u Do not put your hands in the hot fluid. u Do not carry, shift, tip or otherwise move the heating bath when it is filled with hot fluid. u Do not fill the heating bath right to the very top. Allow for the expansion of the fluid when heated. u Do not switch on the heating bath when it is empty.
6 | Operation BÜCHI Labortechnik AG 6.1.2 Fitting the evaporating flask IMPORTANT Risk of evaporating flask damage if fitted incorrectly u When fitting the evaporating flask make sure that the edge of the glass does not strike the vapor duct. u Tighten combiclip no more than handtight. u Carefully fit evaporating flask (3) onto the vapor duct (2). u Slide clip (4) over the neck of the flask. u Screw combiclip (1) clockwise until handtight.
BÜCHI Labortechnik AG 6.1.3 Operation | 6 Adjusting immersion angle of evaporating flask u Switch off the Rotavapor on the heating bath. u Hold the condenser (1) firmly with one hand and release the lever (2) with the other hand. u Adjust the immersion angle. u Lock the rotary drive unit in position again with the lever (2). u Make sure that there is at least 10 mm clearance between the edge of the heating bath and the evaporating flask or vapor duct.
6 | Operation BÜCHI Labortechnik AG 6.1.4 Fitting the receiving flask Materials required: Grease Glisseal 40 blue (order number 048197) u Apply a thin coat of Grease Glisseal 40 blue to the ground joint of the receiving flask. u Fit the receiving flask (3) onto the condenser from below and secure it with the ball joint clamp (2). 6.1.
BÜCHI Labortechnik AG Operation | 6 Moving the vertical adjustment range up/down CAUTION Risk of injury when adjusting apparatus height u Make sure that your fingers are not trapped when adjusting the apparatus height. u Make sure that all tubing are long enough and are not under strain after making the adjustment. 1 2 3 u Loosen the two screwhandles (2) and (3).
6 | Operation BÜCHI Labortechnik AG 6.2 Performing distillation DANGER Risk of poisoning from inhalation of hazardous vapors Do not inhale any vapors produced during distillation. Ensure that vapors are removed immediately by a suitable fume hood. Only use the device in well ventilated areas. If vapors escape from joints or connections, check the seals concerned and re place them if necessary. u Do not distill any unknown fluids. u Observe the safety data sheets for all fluids used.
BÜCHI Labortechnik AG Operation | 6 u Immerse the evaporating flask in the heating bath (see Chapter 6.2.1 "Raising and lowering the evaporating flask", page 33). u Wait 1 – 2 minutes to make sure distillation starts. u If necessary, adjust the vacuum and/or the heater temperature (see Chapter 6.2.3 "Optimization distillation", page 35). 6.2.
6 | Operation BÜCHI Labortechnik AG 6.2.2 Adjusting distillation conditions To obtain optimum distillation conditions, the energy absorbed by the solvent from the heating bath must be removed again in the condenser.
BÜCHI Labortechnik AG 6.2.3 Operation | 6 Optimization distillation Depending on the solvent involved, it may also be possible to further optimize the dis tillation process. The distillation should always be set up so that the condensate does not cover more than three quarters of the coil in the condenser. The top quarter should remain exposed.
6 | Operation BÜCHI Labortechnik AG u In applications where no vacuum is applied, lower the temperature of the heating bath. That will cause less solvent to evaporate. 6.2.4 Feeding solvent during distillation Precondition: R An external vacuum pump is connected and running. R A feed tubing leading from the glass stopcock to the evaporating flask is fitted. u Connect a supply tubing (2) for the solvent to the glass stopcock (1) and hold it in the solvent.
BÜCHI Labortechnik AG 6.3 Operation | 6 Finishing distillation u Raise the rotary drive unit (see Chapter 6.2.1 "Raising and lowering the evaporat u u u u u u u u u 6.3.1 ing flask", page 33). Vent the Rotavapor. Turn off the rotary drive unit (set the rotation speed to 0 rpm). Switch off the heating bath CAUTION! Risk of skin burns from hot evaporating flask. Check the tempera ture of the evaporating flask and, if necessary, allow it to cool down or else wear suitable protective gloves.
6 | Operation BÜCHI Labortechnik AG 6.3.2 Removing the receiving flask u Raise the rotary drive unit (see Chapter 6.2.1 "Raising and lowering the evaporat ing flask", page 33). u Vent the Rotavapor. u Turn off the rotary drive unit (set the rotation speed to 0 rpm). u Firmly hold the receiving flask (3), remove the ball joint clamp (2) and remove the receiving flask. u Make sure that any dripping condensate cannot cause any damage.
BÜCHI Labortechnik AG 7 Cleaning and servicing | 7 Cleaning and servicing NOTE Users may only carry out the servicing and cleaning operations described in this sec tion. Any servicing and repair work which involves opening up the housing may only be carried out by BUCHI service technicians. u Use only genuine BUCHI consumables and spare parts in order to ensure correct operation of the device and preserve the warranty. u . 7.1 Inspecting and cleaning the vapor duct 1 2 u Switch off the device.
7 | Cleaning and servicing 7.3 BÜCHI Labortechnik AG Checking seals Seals are wear parts. They have to be regularly inspected, cleaned and, if necessary, replaced. The life of a seal depends on much it is used and how well it is looked after. 1 2 3 4 5 1 Vacuum connection seal 4 Feed tubing seal 2 Coolant seal 5 Vacuum gasket (not visible) 3 Coolant seal u Remove seals and inspect for damage and cracks. u Rinse intact seals in water or ethanol and dry with a soft cloth.
BÜCHI Labortechnik AG 7.5 Cleaning and servicing | 7 Cleaning the heating bath IMPORTANT Risk of short circuit from fluid penetration into device u Do not immerse heating bath or rotary drive unit in water or pour water over them. u Only wipe down the housing with a damp cloth.
8 | Help with faults BÜCHI Labortechnik AG 8 Help with faults 8.1 Faults, possible causes and remedies Fault Possible cause Remedy Device does not work Device is not connected to power supply u Check power supply (see Fuse blown u Replace fuse (see Chapter Chapter 5.6 "Electrical con nections", page 25). 8.2.2 "Replacing the fuse", page 45). u If fault recurs, contact BUCHI Customer Service.
BÜCHI Labortechnik AG Help with faults | 8 Fault Possible cause Optimum distilla Too much backevaporation tion not from the receiving flask (espe achieved cially with solvent mixtures) Other faults in distillation process (e.g. sudden cooling, too little heat flow, etc.) Operation Manual Rotavapor® R100 Remedy u Empty receiving flask and restart distillation (see Chap ter 6.3.2 "Removing the re ceiving flask", page 38, Chapter 6.1.4 "Fitting the re ceiving flask", page 30 and Chapter 6.
8 | Help with faults BÜCHI Labortechnik AG 8.2 Remedy 8.2.1 Resetting overheat safety cutout CAUTION Risk of skin burns from hot components u Do not touch hot components unless wearing suitable protective gloves. u u u u Switch off the device. Unplug the power supply for the heating bath and rotary drive unit. Allow the heating bath to cool down then empty it. Using a narrow object or screwdriver, press the switch (1) on the underside of the heating bath. 5 The overheat safety cutout is reset.
BÜCHI Labortechnik AG 8.2.2 Help with faults | 8 Replacing the fuse The fuse is on the rear of the heating bath. u u u u u u Allow the heating bath to cool down. Disconnect the power cord. Open the fuse holder (1) with a large screwdriver. Replace the blown fuse with an intact one of the same rating. Screw the fuse holder (1) back in. Reconnect the power cord.
9 | Taking out of service and disposal BÜCHI Labortechnik AG 9 Taking out of service and disposal 9.1 Taking out of service u Remove all fluids from the glass components (see Chapter 7.6 "Removing solvent accumulations", page 41). u Switch off the device. u Unplug the power supply for the heating bath and rotary drive unit. u Remove all glass components. 9.2 Disposal The operator is responsible for proper disposal of the Rotavapor®.
BÜCHI Labortechnik AG Appendix | 10 10 Appendix 10.1 Solvent table Solvent Formula Molar Evaporation en Boiling mass in g/ ergy in J/g point in °C mol at 1013 mbar Density in Vacuum in g/cm3 mbar for 40 °C boiling point Acetone CH3H6O 58.1 553 56 0.790 556 nAmyl alcohol, npentanol C5H12O 88.1 595 37 0.814 11 Benzene C 6H 6 78.1 548 80 0.877 236 nbutanol C4H10O 74.1 620 118 0.810 25 Tert butyl alcohol (2 C4H10O methyl2propanol) 74.1 590 82 0.
10 | Appendix BÜCHI Labortechnik AG Solvent Formula Molar Evaporation en Boiling mass in g/ ergy in J/g point in °C mol at 1013 mbar Density in Vacuum in g/cm3 mbar for 40 °C boiling point 1,1,2,2tetra chloroethane C2H2Cl4 167.9 247 146 1.595 20 Carbon tetrachloride CCl4 153.8 226 77 1.594 271 1,1,1trichloroethane C2H3Cl3 133.4 251 74 1.339 300 Tetrachloroethylene C2Cl4 165.8 234 121 1.623 53 THF (tetrahydrofu rane) C 4H 8O 72.1 – 67 0.
BÜCHI Labortechnik AG 10.2.1 Appendix | 10 Glass apparatus V 11055921 040627 11055922 P+G 028606 040625 000636 000646 048237 023875 023900 028096 032339 (STJ 29/32) 032341 (STJ 24/40) 003275 Order no. Description 11057056 Glass assembly V. Vertical condenser, Order no. Description 000646 1460cm² 11055921 Condenser V. Vertical cond., 1460cm² Tubing. PTFE, Ø4.7/5.5mm, transpar ent, 330mm 000636 11057057 Glass condenser V. Vertical cond., Vacuum gasket. KD22, PTFE 028096 Tubing.
10 | Appendix BÜCHI Labortechnik AG 10.2.2 Glass apparatus C 027479 000672 027462 040628 040641 032013 040627 000646 027344 028606 052892 052891 048237 028096 023875 023900 032339 (STJ 29/32) 032341 (STJ 24/40) 003275 000636 Order no. Description Order no. Description 040640 Glass assembly C. Cold trap, 500cm² 040627 Glass stopcock. Standard, glass, SJ18.8/38 040641 Cold trap mantle. For C condenser 038000 Hose barbs, set. 6 pcs.
BÜCHI Labortechnik AG 10.2.3 Appendix | 10 Accessories Heating Bath Heating Bath B100. 2095°C, 220240V 11061895 Heating power: 1300 W, maximum flask size: 4000 mL Allows adjusting set temperature and indicates actual temperature digitally Heating Bath B100. 2095°C, 100120V 11061894 Heating power: 1300 W, maximum flask size: 4000 mL Allows adjusting set temperature and indicates actual temperature digitally Accessories for heating bath Top cover.
10 | Appendix BÜCHI Labortechnik AG Water regulation nozzle. Restriction valve, hose clamp, sieve Used when tap water is applied as vacuum source, to reduce flowrate of the water 011606 Water jet pump. Plastic Used when tap water is applied as the vacuum source 002913 Water jet pump, B764. Magnetic valve, FFKM, 24V 031358 Simple principle of vacuum generation, without cooling water valve, only used in combination with a vacuum controller/interface Water jet pump, B767.
BÜCHI Labortechnik AG Appendix | 10 Glass, SJ24/40, 2000mL 008765 Glass, SJ24/40, 2000mL, P+G 025262 Glass, SJ24/40, 250mL 008754 Glass, SJ24/40, 3000mL 008767 Glass, SJ24/40, 3000mL, P+G 025263 Glass, SJ24/40, 4000mL 047990 Glass, SJ24/40, 4000mL, P+G 047992 Glass, SJ24/40, 500mL 008758 Glass, SJ24/40, 500mL, P+G 025261 Glass, SJ24/40, 50mL 008750 Glass, SJ29/32, 1000mL 000435 Glass, SJ29/32, 1000mL, P+G 020729 Glass, SJ29/32, 100mL 000432 Glass, SJ29/32, 100mL, P+G 033404 Gla
10 | Appendix BÜCHI Labortechnik AG Glass, SJ29/32, 1500mL, for evaporation 034230 Glass, SJ29/32, 500mL, for drying 034767 Glass, SJ29/32, 500mL, for evaporation 034764 Receiving flasks Glass, BJ35/20, 1000mL 000425 Glass, BJ35/20, 1000mL, P+G 020728 Glass, BJ35/20, 1000mL, P+GLT Application temperature: 70 to 40 °C 040775 Glass, BJ35/20, 1000mL, P+G, drain valve 036919 Glass, BJ35/20, 100mL 000422 Glass, BJ35/20, 2000mL 000426 Glass, BJ35/20, 2000mL, P+G 025265 Glass, BJ35/20, 2000
BÜCHI Labortechnik AG 10.2.4 Appendix | 10 Glass, SJ24/40, incl. 20mL zyl. flask (20pcs) 011578 Glass, SJ24/40, incl. 50mL flask (5pcs) 011574 Glass, SJ29/32, incl. 100mL flask (5pcs) 001333 Glass, SJ29/32, incl. 20mL zyl. flask (12pcs) 001335 Glass, SJ29/32, incl. 20mL zyl. flask (20pcs) 001336 Glass, SJ29/32, incl. 20mL zyl. flask (6pcs) 001334 Glass, SJ29/32, incl.
10 | Appendix BÜCHI Labortechnik AG Cap nuts, set. 10pcs, cap nuts with hole, GL14 10.2.5 56/60 041956 Spare parts Drain disc. PTFE, Ø5.1/14mm 040625 Top cover. For C condenser, PETP 027479 Seal, set. For C/CR condenser, PTFE, EPDM 027462 Screw couppling, set. Couppling, pressure spring 048237 Rubber band. To fasten condenser 032013 Cross sleeve. To fasten condenser Not included: Rubber band (032013) 027344 Condenser C. Cold trap, 500m2 040645 Condenser V.
BÜCHI Labortechnik AG 10.3 10.
10 | Appendix BÜCHI Labortechnik AG 10.
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