Operation Manual Rotavapor ® R�210/215 093076 en
Table of contents Table of contents 1 2 3 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 1.1 Reference documents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 1.2 Trademarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 1.3 Abbreviations . . . . . . . . . . . . . . . . .
Table of contents 4 5 6 4 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .25 4.1 Functional principle of a Rotavapor . . . . . . . . . . . . . . . . . . . . . . . . . . .25 4.1.1 Functional principle considering the V assembly as example . . . . . . . . . . . . . .25 4.1.2 Controls of Rotavapor R-210/215 . . . . . . . . . . . . . . . . . . . . . . . . . .
Table of contents 7 8 9 10 11 5 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49 7.1 Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49 7.2 Tube connections and joints . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49 7.3 Sealing system . . . . . . . . . . . . . . . . . . .
1 1 About this manual About this manual This manual describes the Rotavapor and provides all information required for its safe operation and to maintain it in good working order. It is addressed in particular to laboratory personnel and operators. NOTE The symbols pertaining to safety (WARNINGS and ATTENTIONS) are explained in chapter 2. 1.
2 2 Safety Safety This chapter points out the safety concept of the instrument and contains general rules of behavior and warnings from hazards concerning the use of the product. The safety of users and personnel can only be ensured if these safety instructions and the safetyrelated warnings in the individual chapters are strictly observed and followed. Therefore, the manual must always be available to all persons performing the tasks described herein. 2.
2 2.4 Safety Warning notices used in this manual WARNING Generally, the triangular warning symbol indicates the possibility of personal injury or even loss of life if the instructions are not followed. WARNING Hot surface. WARNING Electrical hazard. WARNING Biohazard. ATTENTION With the general “Read this” symbol, ATTENTIONs indicate the possibility of equipment damage, malfunctions or incorrect process results, if instructions are not followed. NOTE Useful tips for the easy operation of the instrument.
2 Safety WARNING Potential explosion risk if solvent vapors accumulate within the instrument housing. • Always use the instrument in a well ventilated area. • Beware of damaged or cracked glass parts. • Beware of the fire hazard. 2.5.2 Other hazards WARNING Certain solvents in or in the vicinity of the Rotavapor can form peroxides and/or are highly inflammable. • A lways be aware of the explosion risk when working with hazardous substances or with substances of unknown composition.
2 Safety Optional • P +G is a unique protective layer for glass components. It offers improved mechanical damage resistance and increases protection against broken glass. It also makes sure that the solvent in the receiving flask is not spilling, if the flask is damaged. • The protective shield (optional accessory) protects operators from broken glass, solvent splashes and hot heating medium in case of accidents or an implosion. • With the support rod the condenser can additionally be clamped. 2.
3 3 Technical data Technical data This chapter introduces the reader to the instrument specifications. It contains the scope of delivery, technical data, requirements and performance data. 3.1 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. 3.1.
3 Technical data Order number: 2 3 1 x x x x x x Rotavapor R-215 The vapor temperature sensor is comprised in the scope of delivery of the condensers V, S, and E. Order number: 2 3 2 x x x x x x Rotavapor R-210 without heating bath x x x x Rotavapor R-215 without heating bath x x x x Rotavapor R-210/215 230 V 50/60 Hz x x x x Rotavapor R-210/215 100–120 V 50/60 Hz Order number: 2 3.1.
3 Technical data Order number: 2 3 x x 1 x x x x Vapor duct SJ 29/32 x x x x Vapor duct SJ 24/40 x x x x Vapor duct SJ 29/42 A x x x Glass assembly A Order number: 2 3 x x 2 Order number: 2 3 x x 3 Order number: 2 3 x x x • • • • Diagonal condenser Can be used where height is limited For standard distillations Evaporating flask feed via stop-cock Order number: 2 3 x x x V x x x Glass assembly V • • • • • • 13 Vertical condenser Needs little space For st
3 Technical data Order number: 2 3 x x x C x x x Glass assembly C • Dry ice condenser • For distillation of solvents with low boiling points • Evaporating flask feed via stop-cock • No cooling water necessary • Maximum condensation due to low temperatures Order number: 2 3 x x x S x x x Glass assembly S • • • • • 14 Vertical condenser with shut-off valve For distillations also with reflux Evaporating flask feed via stop-cock Connection for vapor temperature sensor Auto distillatio
3 Technical data Order number: 2 3 x x x E x x x Glass assembly E • Descending condenser with expansion vessel • Ideal for distillations exhibiting foaming or bumping • Evaporating flask feed via stop-cock • Connection for vapor temperature sensor Order number: 2 3 x x x R x x x Glass assembly CR • Dry ice condensation • For the distillation of solvents with low boiling points also with reflux • Evaporating flask feed via stop-cock • No cooling water necessary • Maximum condensation
3 Technical data Order number: 2 3 x x x Y x x x Glass assembly BY • V ertical condenser with additional double jacket for cooling • Additional joint on the top of the condenser for flexible expansion • For particularly efficient condensation • Evaporating flask feed via stop-cock • Connection for vapor temperature sensor Order number: 2 3 x x x x 1 x x P+G coating If required, all glass parts can be plastic coated NOTE The broken flask shown on the picture on the left demonstrates t
3 Technical data Order number: 2 3 x x x x x 1 x x x 2 x Vacuum Controller V-850, 100–230 V 50/60 Hz Order number: 2 3 x x x Vacuum Controller V-855, 100–230 V 50/60 Hz The Auto-distillation probe is comprised in the scope of delivery of the condensers V and S.
3 Technical data Order number: 2 3 x x x x x x 2 Valve unit Table 3-1: Standard accessories Product Order number Cooling water tube silicone 9/6 mm 04133 2 power cords – Type CH plug type 12 or PNE, 2.
3 3.1.
3 Technical data Table 3-2: Optional accessories (cont.
3 Technical data Table 3-2: Optional accessories (cont.
3 3.1.4 Technical data Upgrade Table 3-3: Upgrade R-210 to R-215 - optional Product Order number Upgrade R-210 to R-215, display for rotation speed and vapor temperature (without probe) 48376 Note: Only to be installed by a BUCHI service engineer. 1 sensor for measuring the vapor temperature (only with R-215 and with glass assembly V + S + E) 3.
3 3.
3 3.4 Technical data Solvent table Table 3-6: Solvent table Solvent Formula Molar mass Evaporation energy Boiling point Density in Vacuum in mbar for in g/mol in J/g at 1013 mbar g/cm3 boiling point at 40 °C Acetone CH3H6O 58.1 n-amylalcohol, n-pentanol 553 56 0.790 556 C5H12O 88.1 595 37 0.814 11 Benzene C6H6 78.1 548 80 0.877 236 n-butanol C4H10O 74.1 620 118 0.810 25 tert. butanol (2-methyl-2-propanol) C4H10O 74.1 590 82 0.
4 4 Description of function Description of function This chapter explains the basic principle of the instrument, shows how it is structured and gives a functional description of the assemblies. 4.1 Functional principle of a Rotavapor 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 evaporating flask under vacuum.
4 Description of function c Cooling area The solvent vapor flows very quickly into the condenser. Here, the energy in the solvent vapor is transferred to the cooling medium (mostly water), so that the solvent condenses. d Receiving flask The receiving flask collects the condensed solvent. Vacuum The vacuum reduces the boiling temperature and thus increases the distillation performance.
4 4.1.3 Description of function Rear connections of the Rotavapor 2 1 a Power supply for Rotavapor b Socket for control cable to the vacuum controller (RS-485) or the Vacuum Pump V-700/710 (to be used alternatively) c Socket for vapor temperature sensor d Power supply for heating bath 3 4 Fig. 4.3: Rear connections of the Rotavapor 4.2 Motorized quick-action jack 1 With the motorized quick-action jack, the evaporating flask can be lowered into, and raised from, the water bath.
4 4.3 Description of function Heating bath The heating bath B-491 is multifunctional and can be used as a water bath or as an oil heating bath up to 180 °C. The Heating Bath B-495 can be used as water bath up to 95 °C. If you use a water bath, which is not suitable for the operation above 100 °C only water may be used as heating medium (the use of any type of oils is not allowed). In case of an oil bath (e.g. B-491) only specially approved heating bath liquids may be used.
4 4.5 Description of function Vapor temperature sensor Fig. 4.7: Vapor temperature sensor The vapor temperature sensor measures the temperature of the vapor entering the condenser. This temperature is displayed on the display for vapor temperature and rotation speed (only with R-215). Fig. 4.8: Vapor temperature display at the R-215 4.
4 4.7 Description of function Valve unit If using the Rotavapor without the Vacuum Pumps V-700/710, or with a vacuum controller other then the V-850/855, the valve unit shuts off the connection of the vacuum source when the set point of the vacuum controller is reached. Also, the valve unit serves as a separator to collect small amounts of liquid that may have condensed in the vacuum tubing thereby protecting the pump against contamination. Fig. 4.10: Valve unit 4.
4 4.10 Description of function Infrared interface a Receiver b Transmitter 1 2 Fig. 4.12: Infrared interface The infrared interface transmits heating bath data to the controller. An interruption of the communication with the interface does not affect the process. Function of the infrared interface: • Transmits the current heating bath temperature to enable working with the solvent table. • Reads out the heating bath data (set/actual temperature) and transmits them to the Rotavapor.
5 5 Putting into operation Putting into operation 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 immediately 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.
5 Putting into operation Saving energy For heating baths there are various ways to save energy. By using floating balls in the water bath, evaporation of water is reduced. As a result, the bath heating has to switch on less often. This measure helps to save up to 50 % of energy. At the same time approximately 70 % less water is used. Additionally, a cover is available to put over the heating bath during operation which also saves energy between distillations. Fig. 5.
5 4 5 3 Putting into operation a Water inlet b Water outlet c Water level indication d Level adjustment for the replenishment e Overflow Connect the feeding water hose to the hose connection for the water inlet a. Position c indicates the water level within the heating bath and can be adjusted by pulling up or down the level adjustment tube d. Thus, the overflow in the cylinder e is moved up or down and therewith changes the water level within the heating bath by means of the corresponding tube.
5 5.4 Putting into operation Glass assembly To install the glass assembly, consider the following: • T o fasten the flanges you do not have to remove the flange screwed connection (position e in Fig. 5.3). Just open the flange screwed connection wide enough, so that the flange can be pushed through. • You can also secure the glass assemblies V, S, C, E, CR, BY using the corresponding optional support rod. • Secure the receiving flask with the clip provided for this purpose.
5 5.6 Putting into operation Installing the reflux insert 1 2 3 4 5 To install the reflux insert, proceed as follows: • Take the standard flange screwed connection off the drive unit. • Fix the gasket WD 26 (seal) (position 3) to the reflux insert (position 2). • Mount the reflux insert onto the drive unit. • Mount the flange srewed connection (position 1) without tightening it. • Check whether the O-ring (position 5) is positioned properly within the reflux insert.
5 5.8 Tube connections 5.8.
5 5.8.2 Putting into operation Cooling water tubes When connecting the white cooling water tubes, consider the following: • Use tube clips GL-14. • The tubes used must all have the same inner diameter (approximately 6 mm). • For safety reasons, secure the tubes with commercial tube pivoting clamps or cable binders. • To save cooling water, you can use the Distillation Chiller F-1xx. • Check the tubes from time to time and replace them when they are brittle. Fig. 5.9: Cooling water tubes 5.8.
5 5.8.4 Putting into operation Tube connections to the valve unit To connect the valve unit electrically, proceed as follows: • Connect the connection “1” of the valve unit to the glass assembly of the Rotavapor. • Connect the “Pump” connection of the valve unit to the pump inlet. • Connect the “CONTR” connection of the valve unit to the vacuum controller. NOTE When the tube clip to an additional instrument is not used, close it with a screw cap.
5 5.9 Putting into operation Installing the vacuum controller To install the vacuum controller on the Rotavapor, proceed as follows: • Screw the holder a for the vacuum controller to the top of the Rotavapor. • Slide the guide rail b of the vacuum controller over the holder. • Fix the vacuum controller to the holder by tightening the wing nut c. 3 2 1 Fig. 5.12: Installing the vacuum controller 5.
5 5.11 Putting into operation Installing the vapor temperature sensor 1 To measure the vapor temperature during operation, the vapor temperature sensor must be connected. For this purpose: • Plug it into the socket at the rear of the R-215 a (with an R-210 this is not possible). • Introduce the sensor into the corresponding opening in the condenser and tighten it with the GL-14 screw. Fig. 5.14: Vapor temperature sensor 5.
6 6 Operation Operation This chapter explains the operating elements and possible operating modes. It gives instructions on how to operate the Rotavapor properly and safely. ATTENTION Check the glassware for damages prior to each operation and use only glassware in perfect condition. Glassware with cracks, stars or other damages can break during operation. 6.1 Settings at the heating bath 6.1.
6 6.1.3 Operation Switching the B-491 from oil bath mode to water bath mode To switch the heating bath from oil bath mode to water bath mode, proceed as follows: • Switch off the heating bath. • Turn the adjusting knob to any position except for 0 °C or 180 °C. • Switch on the heating bath. • As soon as the temperature is indicated on the display, turn the knob to the 0 °C position within 3 seconds. The indication “WATER” will now appear on the display. Fig. 6.
6 6.2 Operation Immersion angle of the evaporating flask into the heating bath 1 2 3 The immersion angle into the heating bath is, by default, set to 30°. If you need to operate with another angle, e.g. when operating with a small flask, the angle can be changed as follows: • Turn off the instrument. • Hold the glass assembly a with the one hand and loosen the anchoring c with the other hand by pulling the knob.
6 6.3 Operation Lowering and raising the evaporating flask into and out of the heating bath The stop-position of the quick-action jack can be adjusted so that neither the vapor tube, the manifold, or the Combi Clip touch the bottom or edge of the bath and a desired immersion depth of the evaporation flask in the heating bath is achieved. To adjust the stop-position of the quick-action jack, proceed as follows: • Push the button a up or down to move the quick-action jack to the desired position.
6 Operation Δ T2 (min. 20 °C) Δ T1 (min. 20 °C) Fig. 6.5: 20-40-60 ° rule 6.5 Distilling To start operating the instrument, the following conditions have to be fulfilled: • All electrical connections are established correctly. • All sealings are inserted correctly. • All joints are greased. To start operating the instrument, proceed as follows: • Switch on the instrument. • Allow cooling water with a temperature not higher than 20 °C to flow through the condenser at approx. 40–50 l/h.
6 Operation ATTENTION Risk of overflowing. • W hen you are operating with a 5 l heating bath, make sure that the controller is configured in a way that the flask is not automatically submerged into the heating bath to avoid an overflowing of the heating bath due to displacement. Introduce the flask manually instead. • A fter the set vacuum has been reached, wait for about 1–2 minutes to see whether distillation begins.
6 6.7 Operation When the distillation “dies out” When the distillation “dies out”, 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.
7 7 Maintenance and repairs Maintenance This chapter gives instructions on all maintenance work to be performed in order to keep the instrument in good working condition. WARNING All maintenance and repair work requiring the opening or removal of instrument covers may only be carried out by trained personnel and with the tools provided for this purpose. WARNING Electrical hazard: • P rior to all maintenance work on the instrument switch off the power supply and remove all sources of flammable vapor.
7 7.3.1 Maintenance and repairs 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 solft cloth. To remove the seals, see chapter 5.5, Installing the condenser and the seal. 7.3.2 Replacing the seals After 3 - 12 months, depending on the wear, the seals should be replaced.
8 8 Troubleshooting 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 troubleshooting 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”.
8 Troubleshooting Table 8-1: General malfunction and their remedy Sealing system has been installed incorrectly Check sealing system Seal is defective Replace seal Table 8-2: Malfunctions with vacuum controller and vacuum pump and their remedy Malfunction Possible cause Corrective measure Frequent switching of valve or pump System is leaky Check all sealing points (tubes and their connections) Choosen hysteresis is too small Choose larger hysteresis (if endvacuum is higher than 700 mbar, switch
8 Troubleshooting Table 8-4: Error messages Rotavapor Error number Displayed at Possible cause Remedy E10 R-215 Lift error (excess temperature on the PCB or motor current too high) Contact the BUCHI customer service E11 Error is read out via the RS-485 interface and can be read out at the vacuum controller The EEPROM of the Rotavapor contains inconsistent data or is defective Contact the BUCHI customer service E12 Error is read out via the RS-485 interface and can be read out at the vacuum co
8 8.2 Troubleshooting Customer service Only authorised service personnel are allowed to perform repair work on the instrument. These persons have a comprehensive technical training and knowledge of possible dangers which might arise from the instrument. Addresses of official BUCHI 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 application problems, contact one of these offices.
9 9 Shutdown, storage, transport and disposal Shutdown, storage, transport and disposal This chapter instructs how to shut down the instrument, how to pack it for storage or transport, and specifies the storage and shipping conditions. 9.1 Storage and transport WARNING Biohazard: • Remove all dangerous substances from the instrument and clean it thoroughly. Store and transport the instrument in its original packaging.
9 9.3 Shutdown, storage, transport and disposal 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.
10 10 Spare parts Spare parts This chapter lists spare parts, accessories, and optional extras, including all of the relevant order information for ordering from BUCHI. Always state the product designation and part number when ordering any spare parts. Use only genuine BUCHI consumables and spare parts for maintenance and repair to ensure optimum system performance and reliability. Prior written permission of the manufacturer should be obtained before any modifications are made to the spare parts used.
10 10.1 Spare parts Glass assembly A Fig. 10.1: Glass assembly A Table 10-1: Glass assemblies A Product Order number Product Order number Glass assembly A05 complete, with 1 l receiving flask, without seal and vapor duct 48168 PTFE drain disk 40625 Diagonal condenser A 05 (23875+23900 + Tube clips GL-14 complete) 46988 Stop cocks SJ 18.
10 10.2 Spare parts Glass assembly V Fig. 10.2: Glass assembly V Table 10-2: Glass assemblies V Product Order number Product Order number Glass assembly V complete with 1 l receiving flask without, seal and vapor duct 40600 PTFE drain disk 40625 V condenser (23875 + 23900 + tube clips GL-14 complete) 40601 Stop cocks SJ 18.
10 10.3 Spare parts Glass assembly C Fig. 10.
10 Spare parts Table 10-3: Glass assemblies C Product Order number Product Order number Glass assembly C05 complete with 1 l receiving flask, without seal and vapor duct 40640 Stop cocks SJ 18.
10 10.4 Spare parts Glass assembly S Fig. 10.
10 Spare parts Table 10-4: Glass assemblies S Product Order number Product Order number Glass assembly S complete with 1 l receiving flask, without seal and vapor duct 40650 Shut-off tab 40626 Vertical condenser S, including tube clips GL-14 complete 40651 Stop cocks SJ 18.
10 10.5 Spare parts Glass assembly CR Fig. 10.
10 Spare parts Table 10-5: Glass assemblies CR Product Order number Product Order number Glass assembly CR complete with 1 l receiving flask (without reflux insert 48080) 40670 Stop cocks SJ 18.8/38 40627 Cold trap CR outer part (including tube clips GL-14 complete) 11228 Stop cocks SJ 18.
10 10.6 Spare parts Glass assembly E Fig. 10.
10 Spare parts Table 10-6: Glass assemblies E Product Order number Product Order number Glass assembly E complete with 1 l receiving flask, including support rod E (without reflux insert 48080) 40660 Support rod E complete (optional) 48181 Glass assembly E P+G complete with 1 l receiving flask (without reflux insert 48080) 40662 Tube clips GL-14, bent, complete, set of 4 37287 U tube (including 40624) 01003 PTFE tube 300 mm 00646 U tube P+G (including 40624) 33508 Reflux insert, complete
10 10.7 Spare parts Glass assembly BY Fig. 10.
10 Spare parts Table 10-7: Glass assemblies BY 10.
10 10.
10 Spare parts Table 10-13: Vapor ducts short for condenser V, C, S, E, CR, BY Standard joints without Combi Clip with Combi Clip SJ 24/40 48067 48161 SJ 29/32 46962 48160 SJ 29/42 48069 48162 SJ 34/35 48073 48163 Combi clip, complete 40620 Table 10-14: Vapor ducts for analytical applications for condenser V, C, S, E, CR, BY Standard joints without Combi Clip with Combi Clip SJ 29/32 50560 SJ 24/40 50561 SJ 29/42 50562 SJ 34/35 50563 Table 10-15: Condenser holder Product Ord
10 Spare parts Table 10-17: Receiving flask Content uncoated P+G P+G low temperature 50 mL 00421 100 mL 00422 250 mL 00423 500 mL 00424 25264 40774 1000 mL 00425 20728 40775 2000 mL 00426 25265 40776 3000 mL 00427 25266 40777 Beaker flask For working with high viscosity or solid substances. The large opening allows for smooth draining and cleaning. Foaming solutions can be processed more easily. Filling volume: 1.5 l version = 500 mL 0.
10 Spare parts Table 10-20: Distillation spider with 5 flasks Content Order number 50 mL with SJ 24/29 01332 100 mL with SJ 24/29 01333 Table 10-21: Reitmeyer trap for slightly foaming solutions Product Order number SJ 29/32 36576 SJ 24/40 36577 10.
10 Spare parts Table 10-25: Cover Product Order number Top cover B-491 48230 Table 10-26: Water control valve ½” Product Order number Water control valve ½” complete 11606 Table 10-27: Heating Bath B-495 Product Order number Level adjustment tube for bath replenishment, complete 48335 O-ring 48339 Table 10-28: Base plate Product Order number Base plate B-491 for R-210/215/R II, 230 V 48268 Base plate B-491 for R-210/215/R II, 100-120 V 48269 Table 10-29: Cooling water valve 1 2 3 74
10 Spare parts Table 10-31: Control/communication cables Product Order number Control cable between vacuum controller and Vacuum Pump RJ 45, 330 mm (speed control) 44288 Control cable for Vacuum Controller V-500/V-1000, compatible with Vacuum Controller V-800/805 38010 Control cable between Rotavapor and Vacuum Pump RJ 45, 2000 mm (speed control) 44989 Support set for vacuum controller/ manometer with needle valve for R-210/215, V-700/710 47280 Table 10-32: Glisseal laboratory grease Product Or
11 11 Declarations and requirements 11.1 FCC requirements (for USA and Canada) Declarations and requirements English: This equipment has been tested and found to comply with the limits for a Class A digital device, pursuant to both Part 15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communications. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment.
11 11.
