Operation Manual Rotavapor R II ® 093102 en
Table of contents Table of contents 1 2 3 4 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.1 Reference documents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.2 Trademarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.3 Abbreviations . . . . . . . . . . . . . . . .
Table of contents 5 6 7 8 9 10 11 4 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 5.1 Installation site . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 5.2 Electrical connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 5.3 Commissioning the heating bath . . . . . . . . . . .
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.
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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, ATTENTION 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. • Always 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 4 x 2 x x Vapor duct SJ 24/40 Order number: 2 4 x x A x Glass assembly A • • • • Diagonal condenser Can be used where height is limited For standard distillations With optional tap for continuous feeding Order number: 2 4 x x V x Glass assembly V • • • • 12 Vertical condenser Minimum space requirement For standard distillations With optional tap for continuous feeding R II Operation Manual, Version E
3 Technical data Order number: 2 4 x x C x Glass assembly C • Dry ice condenser • For distillation of solvents with low boiling points • With optional tap for continuous feeding • No cooling water necessary NOTE The condenser mounting (040607 and 040608) in combination with glass assembly A is not included in the basic instrument.
3 3.1.2 Technical data Standard accessories Table 3-1: Standard accessories Product Order number Cooling water tube silicone 9/6 mm 2 power cords 004133 – Type CH plug type 12 or PNE, 2.5 m 010010 Type Schuko 010016 Type GB 017835 Type AUS 017836 Type USA 010020 4 cable binders – Operation Manual: 3.1.
3 Technical data Table 3-2: Optional accessories (cont.
3 Technical data Table 3-2: Optional accessories (cont.
3 3.
3 3.
3 3.4 Technical data Solvent table Table 3-5: Solvent table Solvent Acetone n-amylalcohol, n-pentanol Benzene n-butanol, tert.
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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 a Evaporation area The solvent is heated by means of a heating bath. A thin solvent film forms on the inside of the rotating evaporating flask, resulting in an increased evaporation rate. The rotations also lead to an even mixing of the sample thus preventing stationary overheating in the flask. b Rotation drive including vapor duct The drive unit ensures that the evaporating flask rotates evenly.
4 4.1.2 Description of function Controls of Rotavapor R II a Mains switch of Rotavapor b Knob for rotation speed c Combi-Clip for easy flask/vapor duct removal d Lock button to block the drive unit e Heating bath handle f Heating LED g Adjusting knob for heating bath temperature h Mains switch for heating bath i Quick-action jack to raise and lower the evaporating flask j Knob for immersion angle adjustment Fig. 4.
4 4.1.3 Description of function Rear connections of the Rotavapor a Power supply of Rotavapor b Power supply of heating bath Fig. 4.3: Rear connections of the Rotavapor 4.2 Quick-action jack With the quick-action jack, the evaporating flask can be lowered into and raised from the water bath. Turn the handle a to the left-hand side and press it up or down. 1 Fig. 4.
4 4.3 Description of function Heating bath The heating bath can be used as a water heating bath up to 95 °C. a Power supply of heating bath b Mains switch (splash water protected) c Adjusting knob for setting the bath temperature d Heating LED e Handle for easy transport and movement 5 4 1 2 3 Fig. 4.5: Heating bath next to the base plate 4.
4 4.5 Description of function Protective shield (optional) The protective shield protects the user from splashes of heating medium when the flask is rotating and from pieces of broken glass in the unlikely event of an implosion of the evaporating flask. Fig. 4.7: Protective shield 4.6 Woulff bottle The Woulff bottle serves as safety vessel between the Rotavapor and the vacuum pump. In case of an impure distillation the condensate is collected in the Woulff bottle and thus cannot reach the pump. Fig.
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 5.5 Putting into operation Installing the condenser and the seal When installing the condenser and mounting the seal, consider the following order: • Insert the vapor duct c until a click sound is heard. • Fix the seal b to the condenser a. • Screw on the condenser with the flange screwed connection e (normally, the flange screwed connection must not be removed). • Screw the Combi-Clip d onto the vapor duct. Fig. 5.3: Exploded view of condenser and seals 5.
5 Putting into operation ATTENTION The support rod is not designed to carry the weight of the glass assembly on its own. Its sole purpose is to stop the glass assembly tilting forward or backwards when the flanged coupling is released. 5.7 Tube connections 5.7.1 Connection scheme a Vacuum connection to valve unit or Woulff bottle b Cooling water connections Fig. 5.5: Tubing scheme 5.7.
5 5.7.3 Putting into operation Vacuum tubes When connecting the red vacuum tubes, proceed as follows: • Use tube connections GL 14. • The tubes used must all have the same inner diameter (approximately 5 mm). • Keep vacuum tubes as short as possible. • When you are operating with the new BUCHI Vacuum Controller V-850/V-855 and Vacuum Pump V-700/V-710 connect a Woulff bottle between the vacuum source and the Rotavapor.
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6 6 Operation Operation This chapter explains the operating elements and possible operating modes. It gives instructions on how to operate the instrument properly and safely. WARNING Risk of injury. • Never operate the instrument when glassware is damaged. 6.1 Setting the heating bath temperature ATTENTION As soon as the power plug is connected and the mains switch is turned on, the bath starts heating if the actual temperature is below the set temperature.
6 6.3 Operation Selecting the distillation conditions To achieve optimal distillation conditions, the distillation energy supplied by the heating bath must be removed by the condenser. To ensure this, operate the instrument according to the following rule of thumb: Cooling water: max. 20 °C Vapor: 40 °C Bath: 60 °C How are these conditions achieved?: • Set the bath temperature to 60 °C. • Set the cooling water temperature not higher than 20 °C.
6 6.4 Operation Distilling To start operating the instrument, the following conditions have to be fulfilled: • All electrical connections are established correctly. • All sealing 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 3/4 Fig. 6.3: Optimal condensation area of a condenser 6.6 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.
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: • Prior 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 Seals are subject to wear and tear, thus you should check them regularly and replace them, if necessary, e.g.
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 Malfunction Possible cause Corrective measure 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) Chosen hysteresis is too small Choose larger hysteresis (if endvacuum is higher than 700 mbar, switch to automatic hystere
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.
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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 options including their ordering information. Order the spare parts from BUCHI. Always state the product designation and the part number when ordering spare parts. Use only genuine BUCHI consumables and genuine spare parts for maintenance and repair to assure good system performance and reliability. Any modifications to the spare parts used are only allowed with the prior written permission of the manufacturer.
10 10.1 Spare parts Glass assembly A Fig. 10.
10 10.2 Spare parts Glass assembly V Fig. 10.
10 Spare parts TABLE 10-2: GLASS ASSEMBLIES V Product Order number Combi-Clip 10.3 Product Order number 040621 Set of hose connections bent, GL 14, 4 pieces, 4× olive bent with screw caps 037287 Glass assembly C Fig. 10.
10 Spare parts TABLE 10-3: GLASS ASSEMBLIES C Product 10.
10 Spare parts Table 10-6: SJ Evaporating flask (pear-shaped) Content SJ 29/32 SJ 24/40 SJ 29/42 50 mL 000431 008750 008736 100 mL 000432 008751 008737 250 mL 000433 008754 008738 500 mL 000434 008758 008739 1000 mL 000435 000440 008762 2000 mL 000436 008765 008769 3000 mL 000437 008767 008770 4000 mL 047991 047990 – Table 10-7: SJ Evaporating flask (pear-shaped) P+G Content SJ 29/32 SJ 24/40 SJ 29/42 50 mL 033405 – – 100 mL 033404 – – 250 mL 025520 – –
10 Spare parts Table 10-10: Condenser holder Product Order number Support rod complete 048180 Table 10-11: SJ Drying flask (pear-shaped) Content SJ 29/32 SJ 24/40 500 mL 000452 011579 1000 mL 000453 000420 2000 mL 000454 011580 Table 10-12: Receiving flask (pear-shaped) Content uncoated P+G P+G low temperature 50 mL 000421 – – 100 mL 000422 – – 250 mL 000423 – – 500 mL 000424 025264 040774 1000 mL 000425 020728 040775 2000 mL 000426 025265 040776 3000 mL 000427
10 Spare parts Table 10-13: SJ Beaker flask 1.5 L version Beaker flask Drying flask complete SJ 29,2/32 034230 034269 SJ 24/40 034247 034770 Beaker flask Drying flask 0.5 L version complete SJ 29,2/32 034764 034767 SJ 24/40 034765 034768 Distillation spider SJ 29/32 For simultaneous distillation from a 20 mL cylinder flask. Table 10-14: Distillation spider 20 mL Number of flasks Order number 6× SJ 14.5/23 001334 12× SJ 14.5/23 001335 20× SJ 14.
10 10.6 Spare parts Miscellaneous Floating balls The floating balls form a cover on the water surface, so that the energy consumption is reduced.
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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.
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BÜCHI Labortechnik AG CH-9230 Flawil 1/Switzerland T +41 71 394 63 63 F +41 71 394 65 65 www.buchi.