Buchi Rotavapor R-300 Operation Manual
Below you will find brief information for Rotavapor R-300, B-300 Base, B-301, B-305. The Rotavapor R-300 is a rotary evaporator for efficient and gentle solvent evaporation and condensation under vacuum. It features a rotating evaporating flask, a cooling condenser, and a heating bath (B-301 or B-305) for precise temperature control. The B-300 Base houses the heating bath controls. Different sized heating baths (B-301 and B-305) accommodate various flask sizes. Safe operation is ensured by overheat cut-offs and other safety features.
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Rotavapor® R-300
Operation Manual
Imprint
Product Identification:
Operation Manual (Original) Rotavapor® R-300
11593738
Publication date: 07.2016
BÜCHI Labortechnik AG
Meierseggstrasse 40
Postfach
CH-9230 Flawil 1
E-Mail: [email protected]
BUCHI reserves the right to make changes to the manual as deemed necessary in the light of experience, especially with respect to structure, illustrations and technical detail.
This manual is copyrighted. Information from it may not be reproduced, distributed, or used for competitive purposes, nor made available to third parties. The manufacture of any component with the aid of this manual without prior written agreement is also prohibited.
BÜCHI Labortechnik AG Contents
2.5
2.6
3
3.1
3.2
3.3
2
2.1
2.2
2.3
2.4
Contents
1
1.1
1.2
1.3
1.4
1.5
About this document........................................................................................................... 6
Warning notices in this document........................................................................................................ 6
Symbols ............................................................................................................................................... 6
1.2.1
Warning symbols ..................................................................................................................... 6
1.2.2
Mandatory directive symbols ................................................................................................... 7
1.2.3
Other symbols.......................................................................................................................... 7
Available languages............................................................................................................................. 7
Trademarks.......................................................................................................................................... 7
Trademarks.......................................................................................................................................... 7
3.4
3.5
3.6
4
4.1
4.2
Safety.................................................................................................................................... 8
Intended use ........................................................................................................................................ 8
Use other than that intended ............................................................................................................... 8
Staff qualification ................................................................................................................................. 9
Residual risks ...................................................................................................................................... 9
2.4.1
Dangerous vapors.................................................................................................................... 9
2.4.2
High internal pressure............................................................................................................ 10
2.4.3
Hot surfaces and liquids......................................................................................................... 10
2.4.4
Rotating parts......................................................................................................................... 10
2.4.5
Faults during operation .......................................................................................................... 10
Personal protective equipment .......................................................................................................... 10
Modifications...................................................................................................................................... 10
Product description........................................................................................................... 12
Description of function ....................................................................................................................... 12
Options .............................................................................................................................................. 13
Configuration ..................................................................................................................................... 14
3.3.1
Front view .............................................................................................................................. 14
3.3.2
Rear view ............................................................................................................................... 15
3.3.3
Heating bath user interface.................................................................................................... 16
3.3.4
Type plate .............................................................................................................................. 17
3.3.5
Warning symbols on the device ............................................................................................. 18
3.3.6
Cover for Heating Bath B-305 (optional)................................................................................ 18
Specifications supplied ...................................................................................................................... 19
Technical data ................................................................................................................................... 20
3.5.1
Rotavapor® R-300/R-300 Hand Lift....................................................................................... 20
3.5.2
Heating Bath B-300 Base ...................................................................................................... 20
3.5.3
Heating Bath B-301................................................................................................................ 20
3.5.4
Heating Bath B-305................................................................................................................ 21
3.5.5
Ambient conditions................................................................................................................. 21
3.5.6
Materials ................................................................................................................................ 22
Safety features................................................................................................................................... 23
3.6.1
Overheat cut-out .................................................................................................................... 23
3.6.2
Protection against electrical overload .................................................................................... 23
3.6.3
Clips and holders ................................................................................................................... 23
3.6.4
Glassware .............................................................................................................................. 23
3.6.5
Optional accessories.............................................................................................................. 23
3.6.6
Earthquake safety .................................................................................................................. 23
Transport and storage ...................................................................................................... 24
Transport ........................................................................................................................................... 24
Storage .............................................................................................................................................. 24
Operation Manual Rotavapor® R-300 iii
Contents BÜCHI Labortechnik AG
7
7.1
7.2
7.3
7.4
7.5
7.6
7.7
7.8
5
5.1
Installation.......................................................................................................................... 25
Installation site ................................................................................................................................... 25
5.2
5.3
5.4
5.5
5.6
Securing against earthquakes ........................................................................................................... 25
Fitting the vapor duct, vacuum gasket and cooling condenser.......................................................... 26
Fitting the glass stopcock .................................................................................................................. 27
Fitting PTFE stopcock (optional accessory) ...................................................................................... 28
Fitting the Interface I-300/I-300 Pro (optional accessory).................................................................. 29
5.7
5.8
Mounting VacuBox on R-300 (optional accessory)............................................................................ 31
Mounting LegacyBox on R-300 (optional accessory) ........................................................................ 32
5.9
Fitting the Woulff bottle (optional accessory)..................................................................................... 33
5.10
Fitting AutoDest sensor and vapor temperature sensor (optional accessory) ................................... 34
5.11
Fitting a foam sensor (optional accessory) ........................................................................................ 36
5.12
Connecting vacuum and coolant tubing............................................................................................. 38
5.12.1 Overview: vacuum and coolant tubing ................................................................................... 39
5.13
Setting up the heating bath................................................................................................................ 40
5.14
Fitting the protection shield (optional)................................................................................................ 41
5.15
Connecting the Rotavapor to the power supply................................................................................. 42
5.16
Assembling the BUCHI distillation system......................................................................................... 44
5.16.1 Overview: setting up communication connections ................................................................. 45
5.16.2 Connecting communication cables to the Rotavapor............................................................. 46
5.16.3 Overview: setting up coolant tubing connections................................................................... 47
5.16.4 Overview: setting up vacuum tubing connections.................................................................. 48
5.17
Basic settings..................................................................................................................................... 49
5.18
Quick check ....................................................................................................................................... 50
6
6.1
6.2
6.3
Operation............................................................................................................................ 51
Preparations ...................................................................................................................................... 51
6.1.1
Preparing the heating bath..................................................................................................... 51
6.1.2
Fitting the evaporating flask ................................................................................................... 52
6.1.3
Adjusting immersion angle of evaporating flask..................................................................... 53
6.1.4
Fitting the receiving flask ....................................................................................................... 54
6.1.5
Raising and lowering rotary drive unit.................................................................................... 55
Performing distillation ........................................................................................................................ 59
6.2.1
Operating the Rotavapor without control system (interface).................................................. 60
6.2.2
Operating Rotavapor with Interface I-300/I-300 Pro .............................................................. 61
6.2.3
Adjusting distillation conditions .............................................................................................. 62
6.2.4
Optimization distillation .......................................................................................................... 62
6.2.5
Adding solvent during distillation............................................................................................ 64
Finishing distillation............................................................................................................................ 65
6.3.1
Removing the evaporating flask............................................................................................. 65
6.3.2
Removing the receiving flask ................................................................................................. 66
Cleaning and servicing ..................................................................................................... 67
Inspecting and cleaning the vapor duct ............................................................................................. 67
Checking the system for leaks........................................................................................................... 68
Fitting GL14 union nut with tube seal ................................................................................................ 69
Checking seals .................................................................................................................................. 70
Cleaning the cooling condenser ........................................................................................................ 71
Cleaning the heating bath.................................................................................................................. 71
Cleaning the Woulff bottle.................................................................................................................. 71
Removing solvent accumulations ...................................................................................................... 71 iv Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Contents
8
8.1
8.2
9
9.1
9.2
Help with faults .................................................................................................................. 72
Faults, possible causes and remedies............................................................................................... 72
Resetting safety functions.................................................................................................................. 74
8.2.1
Resetting overheat safety cut-out on heating bath ................................................................ 74
8.2.2
Replacing fuse in heating bath base...................................................................................... 75
Taking out of service and disposal.................................................................................. 76
Taking out of service.......................................................................................................................... 76
Disposal ............................................................................................................................................ 76
10 Appendix ............................................................................................................................ 77
10.1
Solvent table ...................................................................................................................................... 77
10.2
Spare parts and accessories ............................................................................................................. 79
10.2.1 Glass assembly A .................................................................................................................. 79
10.2.2 Glass assembly V .................................................................................................................. 80
10.2.3 Glass assembly C .................................................................................................................. 81
10.2.4 Glass assembly S .................................................................................................................. 82
10.2.5 Glass assembly CR ............................................................................................................... 83
10.2.6 Glass assembly E .................................................................................................................. 84
10.2.7 Glass assembly BY................................................................................................................ 85
10.2.8 Accessories............................................................................................................................ 86
10.2.9 Wear parts ............................................................................................................................. 94
10.2.10Spare parts ............................................................................................................................ 95
10.3
List of abbreviations........................................................................................................................... 98
10.4
Health and safety approval ................................................................................................................ 99
10.5
Health and safety............................................................................................................................. 100
Operation Manual Rotavapor® R-300 v
1 | About this document
1
BÜCHI Labortechnik AG
About this document
These operating instructions describe the Rotavapor® R-300 at the time supplied.
They are an integral part of the product and contain important information that is necessary for safe operation and maintenance.
These operating instructions apply to all variants of the Rotavapor® R-300 and are intended primarily for laboratory staff.
u u u
To ensure safe and trouble-free operation, read these operating instructions before starting up the device and follow the guidance they contain.
Keep the operating instructions somewhere near to the device.
Pass on the operating instructions to any subsequent owner or user.
BÜCHI Labortechnik AG accepts no liability whatsoever for any faults or damage that result from the failure to follow these operating instructions.
u If you still have any questions after reading these operating instructions, please contact BÜCHI Labortechnik AG Customer Service. Contact details for your local agents can be found on the back cover of these operating instructions or on the Internet at http://www.buchi.com.
1.1
Warning notices in this document
Warning notices warn you of dangers that can occur when handling the device. There are four danger levels, each identifiable by the signal word used.
Signal word
DANGER
WARNING
CAUTION
Meaning
Indicates a danger with a high level of risk which could result in death or serious injury if not prevented.
Indicates a danger with a medium level of risk which could result in death or serious injury if not prevented.
Indicates a danger with a low level of risk which could result in minor or medium-severity injury if not prevented.
IMPORTANT Indicates a danger that could result in damage to property.
1.2
1.2.1
Symbols
The following symbols may be displayed in this instruction manual or on the device:
Warning symbols
Symbol Meaning
General warning
Symbol Meaning
Corrosive substance
Dangerous electrical voltage
Biological hazard
Breakable items
Flammable substance
Potentially explosive atmosphere
Dangerous gases
6/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
Symbol Meaning
Hot surface
Risk of hand injury
About this document | 1
Symbol Meaning
Health-harming or irritant substances
Strong magnetism
1.2.2
Mandatory directive symbols
Symbol Meaning
Wear safety goggles
Symbol Meaning
Wear protective clothing
Wear protective gloves Heavy load, do not lift without assistance
1.2.3
1.3
1.4
1.5
Other symbols
NOTE
This symbol draws attention to useful and important information.
R This character draws attention to a requirement that must be met before the instructions below are carried out.
u This character indicates an instruction that must be carried out by the user.
5 This character indicates the result of a correctly carried out instruction.
Available languages
These operating instructions were originally produced in German and have been translated into several other languages. The translations are available on the enclosed CD or can be obtained as a PDF file via http://www.buchi.com.
Trademarks
Product names and registered or unregistered trademarks that are used in this instruction manual are used only for identification and remain the property of the owner in each case.
For example, Rotavapor® is a registered trademark of BÜCHI Labortechnik AG.
Trademarks
Product names and registered or unregistered trademarks that are used in this instruction manual are used only for identification and remain the property of the owner in each case.
For example, Rotavapor® is a registered trademark of BÜCHI Labortechnik AG.
Operation Manual Rotavapor® R-300 7/102
2 | Safety
2
2.1
2.2
BÜCHI Labortechnik AG
Safety
Intended use
The Rotavapor® R-300 is intended for evaporating and condensing solvents. It can be used in laboratories and production facilities for the following operations:
Evaporating solvents
Synthesis and purification of chemicals
Recycling and concentration of solvents
Recrystallization
Drying of powders and granulates
Use other than that intended
Use of any kind other than that described in Chapter 2.1 "Intended use", page 8 and any application that does not comply with the technical specifications (see
Chapter 3.5 "Technical data", page 20) constitutes use other than that intended.
In particular, the following applications are not permissible:
Use of the device in an environment with a potential risk of explosion or areas which require explosion-safe apparatus
Use of the device for processing substances in the food, animal feed or cosmetics industries
Production and processing of substances that can lead to spontaneous reactions, e.g. explosives, metal hydrides or solvents that can form peroxides
Working with explosive gas mixtures
Drying hard, brittle substances (e.g. stone or soil samples) that could damage the evaporating flask
Shock-cooling of the evaporating flask or other glass components
Damage or hazards attributable to use of the product other than as intended are entirely at the risk of the user alone.
8/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
2.3
Safety | 2
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.
They are familiar with the contents of these operating instructions and the applicable safety regulations and apply them.
They are able on the basis of their training or professional experience to assess the risks associated with the use of the device.
Operator
The operator (generally the laboratory manager) is responsible for the following aspects:
The device must be correctly installed, commissioned, operated and serviced.
Only suitably qualified staff may be assigned the task of performing the operations described in these operating instructions.
The staff must comply with the locally applicable requirements and regulations for safe and hazard-conscious working practices.
Safety-related incidents that occur while using the device should be reported to the manufacturer ([email protected]).
BUCHI service technicians
Service technicians authorized by BUCHI have attended special training courses and are authorized by BÜCHI Labortechnik AG to carry out special servicing and repair measures.
2.4
2.4.1
Residual risks
The device has been developed and manufactured using the latest technological advances. Nevertheless, risks to persons, property or the environment can arise if the device is used incorrectly.
Appropriate warnings in this manual serve to alert the user to these residual dangers.
Dangerous vapors
Distillation can produce dangerous vapors that are capable of causing life-threatening toxic effects.
u u u u u u
Do not inhale any vapors produced during distillation.
Ensure that vapors are removed 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 replace them if necessary.
Do not distill any unknown fluids.
Observe the safety data sheets for all fluids used.
Operation Manual Rotavapor® R-300 9/102
2 | Safety
2.4.2
2.4.3
2.4.4
2.4.5
2.5
2.6
BÜCHI Labortechnik AG
High internal pressure
The evaporation of fluids can produce high pressures inside the flask or the condenser. If that pressure becomes too great, the glass components could explode.
u u u
Make sure that the internal pressure inside the glass components is never greater than atmospheric pressure.
When distilling without a vacuum, set the vacuum pump to atmospheric pressure so that excess pressure is automatically dissipated.
If a vacuum pump is not used, leave the vacuum connection open.
Hot surfaces and liquids
The heating bath, evaporating flask and parts of the condenser can become very hot.
If touched they can cause skin burns.
u Do not touch hot surfaces or liquids or else wear suitable protective gloves.
Rotating parts
The evaporating flask and the vapor duct are rotated by the rotary drive unit. Hair, clothing or jewelry can become caught up if allowed to come into contact with the rotating parts.
At high speeds, the heating fluid may be sprayed out by the rotation of the evaporating flask.
u u u u u
Wear work overalls or protective clothing.
Do not wear loose or baggy items of clothing such as scarves or neck-ties.
Tie up long hair.
Do not wear jewelry such as necklaces or bracelets.
At high speeds and/or high temperatures, use the optional safety guard or a similar protective arrangement.
Faults during operation
If a device is damaged, sharp edges, moving parts or exposed electrical wires can cause injuries.
u u u
Regularly check device for visible damage.
If faults occur, switch off the device immediately, unplug the power cord and inform the operator.
Do not continue to use devices that are damaged.
Personal protective equipment
Depending on the application, hazards due to heat and/or corrosive chemicals may arise.
u u
Always wear appropriate personal protective equipment such as safety goggles, protective clothing and gloves.
Make sure that the personal protective equipment meets the requirements of the safety data sheets for all chemicals used.
Modifications
Unauthorized modifications may impair safety and lead to accidents.
u u
Use only genuine BUCHI accessories, spare parts and consumables.
Technical modifications to the device or accessories should only be carried out with the prior written approval of BÜCHI Labortechnik AG and only by authorized
BUCHI technicians.
10/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Safety | 2
BUCHI accepts no liability whatsoever for damage arising as a result of unauthorized modifications.
Operation Manual Rotavapor® R-300 11/102
3 | Product description
3 Product description
3.1
BÜCHI Labortechnik AG
Description of function
The Rotavapor® R-300 is a rotary evaporator with the aid of which single-stage distillation can be carried out quickly without unduly stressing the product. The basis of the process is the evaporation and condensing of solvents in a rotating evaporating flask under vacuum. Distillation under vacuum is more efficient and gentler on the product.
The product is heated in the evaporating flask by the heating bath. The rotary drive unit evenly rotates the evaporating flask. Rotation increases the surface area of the liquid which leads to an increased evaporation rate. This also constantly mixes the product which prevents localized overheating and delayed evaporation.
The vapor passes from the evaporating flask through the vapor duct into the cooling section (cooling condenser). There, the thermal energy of the vapor is transferred to the coolant fluid so that the vapor re-condenses. The resulting solvent is collected in the receiving flask and can then be reused or properly disposed of.
Distillation under vacuum
Distillation capacity depends on the following factors:
Temperature of the heating bath
Pressure in the evaporating flask
Rotation speed of the evaporating flask
Size of the evaporating flask
Pressure in the evaporating flask: a low pressure (below atmospheric) reduces the boiling point of the solvent. A lower boiling point means the solvent does not have to be heated as much. Distillation under vacuum is more efficient and gentler on the product.
Vacuum control: a stable vacuum adapted to the application prevents undesirable solvent emissions and bumping (boiling) of the product. Control of the vacuum is carried out by two means: the BUCHI VacuBox measures the current vacuum in the distillation system. The BUCHI VacuBox is connected to the BUCHI Interface I-300 or
I-300 Pro. The BUCHI Interface is used to display the current readings and control the components of the distillation system. See also Chapter 5.16 "Assembling the BUCHI distillation system", page 44.
Heating bath temperature, coolant temperature and vapor temperature: to ensure optimum distillation, it is important to make sure that the temperature difference between the coolant and the heating bath is at least 40 °C. The temperature of the rising vapor should be mid-way between the heating bath temperature and the coolant temperature. See also Chapter 6.2.3 "Adjusting distillation conditions", page 62.
12/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
3.2
Product description | 3
Options
There are two different heating bath sizes for the Rotavapor® R-300:
The Heating Bath B-301 is suitable for evaporating flasks up to 1 L. See
Chapter 3.5.3 "Heating Bath B-301", page 20.
The Heating Bath B-305 is suitable for evaporating flasks up to 5 L. See
Chapter 3.5.4 "Heating Bath B-305", page 21.
As an additional option, the Rotavapor® R-300 can be operated with the Interface
I-300 or I-300 Pro. Connection of the interface unit to the Rotavapor® requires a
VacuBox.
The Rotavapor® R-300 is available with either manual or motorized vertical adjustment of the rotary drive unit.
Operation Manual Rotavapor® R-300 13/102
3 | Product description
3.3
3.3.1
Configuration
Front view
BÜCHI Labortechnik AG
14/102
4
5
6
2
3
7
8
9
10
11
Fig. 1: Rotavapor R-300 configuration with Heating Bath B-305 and B-301 and Heating Bath
B-300 Base
1 Condenser
2 Glass stopcock
3 Solvent backfeed (tubing)
4 Flange nut
5 Control knob for rotation speed
6 Receiving flask
10 Heating Bath B-300 Base
11 Control knob for heating bath temperature setting
12 On/Off master switch for Rotavapor
13 Button for angle adjustment
14 Locking button for rotary drive unit
15 Combi-clip
7 Handle for height adjustment
8 Heating Bath B-305
9 On/Off master switch for heating bath
16 Evaporating flask
17 Heating Bath B-301
Depending on requirements, either the Heating Bath B-305 (for flasks up to 5 L max.) or the Heating Bath B-301 (for flasks up to 1 L max.) can be used.
Operation Manual Rotavapor® R-300
16
17
12
13
14
15
BÜCHI Labortechnik AG
3.3.2
Rear view
Product description | 3
6
3
4
5
1
2
9
10
Fig. 2: Rear view of Rotavapor R-300
1 Coolant inlet connection 6 Cleaning hole
2 Vapor temperature sensor connection 7 Coolant outlet connection
3 Communication cable connection 8 Vacuum connection
4 Type plate
5 Power supply connection
9 Woulff bottle
10 Vertically adjustable foot for leveling
7
8
Operation Manual Rotavapor® R-300 15/102
3 | Product description
3.3.3
Heating bath user interface
1 on Lift set max.95°
Set
46
°C
50
°C
BÜCHI Labortechnik AG
STOP
3
4
9
5
Fig. 3: User interface of Heating Bath B-300 Base
1 Maximum temperature indication
2 Indication of lift depth stop
3 Actual temperature indication
4 Set temperature indication
6 Set temperature locked indicator
7 Connection symbol – device is being controlled via a BUCHI interface
8 START/STOP function activated on pressing navigation control
9 Control knob for setting required temperature and heater START/STOP function
5 On/Off master switch for heating bath and heating bath base
6
7
8
16/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
3.3.4
Product description | 3
Type plate
The Rotavapor R-300 and the Heating Bath B-301/B-305 each have their own type plate on the rear. On the rear of the Heating Bath B-300 Base there is a fuse rating plate.
BÜCHI Labortechnik AG
CH-9230 Flawil/Switzerland
Type: R-300
SN: 1000000000
Volt: 100 – 240 VAC
Frequ.: 50/60 Hz
Power: 100 W
Built: 2014
Made in Switzerland
1
4
5
6
2
3
7
8
9
11 9 10
Fig. 4: Type plate (example)
1 Company name and address
2 Device name
3 Serial number
4 Input voltage
5 Frequency
6 Maximum power rating
7 Year of manufacture
8 Country of manufacture
9 Approvals
10 Symbol for "Do not dispose of as household waste"
11 Product code
Operation Manual Rotavapor® R-300 17/102
3 | Product description
3.3.5
BÜCHI Labortechnik AG
Warning symbols on the device
The heating bath and the bath cover carry the following warning symbol:
18/102
3.3.6
This symbol warns of the risk of skin burns from the hot surface of the heating bath.
Cover for Heating Bath B-305 (optional)
To save energy and to minimize water evaporation when not in use, a cover is available for the Heating Bath B-305.
1
2
Fig. 5: Heating Bath B-305 with cover
1 Bath cover 2 Heating Bath B-305
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
3.4
Specifications supplied
Product description | 3
Rotavapor® R-300
Heating Bath B-301/B-305
Heating Bath B-300 Base
Cooling condenser
(as per order number)
Vapor duct (with combi-clip)
Vacuum seal (WD26)
Evaporating flask (1 liter)
Receiving flask (1 liter)
Flyer 'List of Solvents'
Required coolant and vacuum tubing
Power cord
System with glassware System without glassware
1
1
1
1
1
1
1
–
1
1
1
1
1
1 set
2
–
1
–
–
1
–
2
Operation Manual Rotavapor® R-300 19/102
3 | Product description
3.5
3.5.1
3.5.2
3.5.3
BÜCHI Labortechnik AG
Technical data
Rotavapor® R-300/R-300 Hand Lift
Dimensions (W x H x D)
Weight
Power supply voltage
Frequency
Power consumption
Enclosure rating
Overvoltage category
Pollution degree
Immersion angle
Vertical adjustment
Vertical adjustment range
Limit position detection adjustment range
Rotation speed range
Lift-out function on power failure
Max. flask capacity
Approval
400 x 615 x 320 mm
13.5 kg
R-300 Hand Lift: 13.0 kg
100 – 240 VAC ± 10 %
50/60 Hz
100 W
IP21
II
2
10 – 50°
Motorized
R-300 Hand Lift: manual
220 mm
170 mm
R-300 Hand Lift: 100 mm
10 – 280 rpm
Yes
R-300 Hand Lift: No
3 kg
CE/CSA
Heating Bath B-300 Base
Dimensions (W x H x D)
Weight
Power supply voltage
Frequency
Fuse rating
183 x 82 x 286 mm
0.8 kg
100 – 120 VAC ± 10 % / 220 – 240 VAC ± 10 %
50/60 Hz
T 12.5 H 250 V (100 – 120 V)
T 6.3 A L 250 V (220 – 240 V)
1500 W Power consumption (with bath)
Enclosure rating
Overvoltage category
Pollution degree
Approval
IP21
II
2
CE/CSA
Heating Bath B-301
Dimensions (W x H x D)
Weight
Power supply voltage
Frequency
218 x 192 x 205 mm
2 kg
100 – 120 VAC ± 10 % / 220 – 240 VAC ± 10 %
50/60 Hz
20/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
3.5.4
3.5.5
Product description | 3
Power consumption
Enclosure rating
Overvoltage category
Pollution degree
Temperature range
Heating medium
0 – 95 °C
Water
Max. evaporating flask size 1 L
Adjustment accuracy ± 1 °C
Regulating accuracy At 60 °C: ± 1 °C
At 95 °C: ± 1 °C
Bath content
Electronic & mechanical overheat cut-out
Approval
1250 W
IP21
II
2
1.8 L
Yes
CE/CSA
Heating Bath B-305
Dimensions (W x H x D)
Weight
Power supply voltage
Frequency
Power consumption
Enclosure rating
Overvoltage category
Pollution degree
Temperature range
Heating medium
Evaporating flask
Adjustment accuracy
Regulating accuracy
Bath content
Electronic and mechanical overheat cut-out
Approval
307 x 202 x 275 mm
4.2 kg
100 – 120 VAC ± 10 % / 220 – 240 VAC ± 10 %
50/60 Hz
1500 W
IP21
II
2
0 – 220 °C
Water/Oil
5 L
± 1 °C
At 60 °C: ± 1 °C
At 95 °C: ± 1 °C
At 180 °C: ± 3 °C
At 220 °C: ± 4 °C
4 L
Yes
CE/CSA
Ambient conditions
Max. altitude above sea level
Ambient temperature
Maximum relative humidity
2000 m
5 – 40 °C
80 % for temperatures up to 31 °C decreasing linearly to 50 % at 40 °C
Operation Manual Rotavapor® R-300 21/102
3 | Product description
3.5.6
BÜCHI Labortechnik AG
The laboratory apparatus described here may only be used indoors.
Materials
Component
Rotavapor casing
Heating bath casing
Heating bath
Protection shield
Protection shield handle
Rotary drive unit
Flange connection to condenser
Seal
Glass components
Material
Aluminum with powder coating
PBT, partially glass-fiber reinforced
Stainless steel 1.4404, glass-peened
PMMA
PBT
Steel 1.4305
Aluminum, anodized
NBR, PTFE coated
Borosilicate 3.3
22/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
3.6
3.6.1
3.6.2
3.6.3
3.6.4
3.6.5
3.6.6
Product description | 3
Safety features
Overheat cut-out
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 cut-out.
The electronic overheat cut-out monitors the temperature limit, the heating rate and the function of the temperature sensor. If the electronic overheat cut-out trips, the device should be inspected by a BUCHI service technician.
The mechanical overheat cut-out consists of a bi-metallic thermostat that immediately cuts off the power supply if the temperature exceeds a certain level. The mechanical overheat cut-out has to be manually reset once the heating bath has cooled down (see Chapter 8.2.1 "Resetting overheat safety cut-out on heating bath", page 74).
Protection against electrical overload
The Heating Bath B-300 Base is fitted with a safety fuse.
The rotary drive unit has an electrical overload cut-out.
Clips and holders
Combi-clip for fixing the evaporating flask and safe release of sticking ground-glass joints
Ball joint clamps for securely fixing the receiving flask
Laboratory stand and holder for fixing glass apparatus
Cap nut for fixing the condenser
Glassware
Inert borosilicate glass 3.3
GL14 hose barbs for preventing glass breakage
Optional feature: P+G plastic-coated glass
Optional accessories
Safety guard to protect user against glass splinters, solvent splashes or hot heating fluid in the event of accidents or implosions
Laboratory stand for providing additional fixing for condenser
For more information, see Chapter 10.2 "Spare parts and accessories", page 79.
Earthquake safety
Lashing eyes for protecting the equipment against falling
For fitting, see Chapter 5.2 "Securing against earthquakes", page 25.
Operation Manual Rotavapor® R-300 23/102
4 | Transport and storage
4 Transport and storage
4.1
BÜCHI Labortechnik AG
Transport
IMPORTANT
Risk of breakage due to incorrect transportation u 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.
Avoid sharp movements during transit.
4.2
u u u
After transportation, check the device and all glass components for damage.
Damage that has occurred in transit should be reported to the carrier.
Keep packing for future transportation.
Storage
u u u
Make sure that the ambient conditions are complied with (see Chapter 3.5
"Technical data", page 20).
Wherever possible, store the device in its original packaging.
After storage, check the device, all glass components, seals and tubing for damage and replace if necessary.
24/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
5 Installation
5.1
Installation | 5
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 fume extraction apparatus available.
Wherever possible, the Rotavapor® R-300 should be set up inside a fume hood. If that is not possible for reasons of space, it can also be set up outside if the safety guard (optional accessory) is fitted and the residual vapors are fed into the fume hood.
5.2
Securing against earthquakes
The Rotavapor R-300 has an earthquake fixing to protect the device against falling.
1
Fig. 6: Earthquake fixing
1 Lashing eye u u u
Lie the Rotavapor R-300 on its back.
Fix the lashing eye (1) to the base of the R-300 from underneath using a screw.
There is a threaded hole provided for the purpose.
Tie the lashing eye to a fixed point using strong cord or a wire.
The Heating Bath B-300 Base can also be secured against earthquakes in similar fashion by fitting a lashing eye on the underneath.
Operation Manual Rotavapor® R-300 25/102
5 | Installation
5.3
BÜCHI Labortechnik AG
Fitting the vapor duct, vacuum gasket and cooling condenser
1
2
3
4
26/102
5
Fig. 7: Fitting vapor duct, cooling condenser and vacuum gasket
1 Cooling condenser
2 Condensate trap
3 Seal
4 Flange nut
5 Vapor duct
NOTE
If the air humidity in the laboratory is high, condensation may form on the outside of the cooling condenser. To catch that condensation, a condensate trap (2) is fitted on the cooling condenser.
NOTE
If at all possible, the ground glass joint of the vapor duct should not be greased.
u Insert vapor duct (5) into the rotary drive unit.
The vapor duct snaps into place with an audible click.
u u
NOTICE! Risk of property damage due to vapor duct falling out if incorrectly fitted.
Pull on the vapor duct to check that it is properly engaged and cannot be pulled out without resistance.
NOTICE! Risk of seal damage if fitted incorrectly.
Insert vacuum gasket (3) into the flange of the cooling condenser (1) as shown.
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Installation | 5 u u u
Fit cooling condenser (1) into the rotary drive unit, keeping it straight as you do so.
When doing so, make sure that the inner lip of the vacuum gasket (3) does not fold over as the vacuum gasket would then be destroyed.
Tighten the flange nut (4) to fix the cooling condenser in position. When doing so, make sure that the spring clip in the flange nut completely encircles the neck of the cooling condenser.
If necessary, fit a tube to carry away the condensation from the condensate trap.
NOTE
For situations in which the equipment is regularly operated at high temperatures, there is a special "high temperature version" of the vapor duct available. Contact
BUCHI Customer Service for further details.
5.4
Fitting the glass stopcock
1
2
3
4
Fig. 8: Cooling condenser with glass stopcock and backfeed tube
1 Glass stopcock
2 Flat face on glass stopcock
3 Glass stopcock handle
4 Solvent backfeed (tubing)
Materials required:
Glisseal 40 red laboratory grease u u u u Feed the tube on the glass stopcock (1) through the vapor duct and into the evaporating flask.
If necessary, connect the backfeed tube for solvent (4).
Coat the ground joint of the glass stopcock with Glisseal 40 red laboratory grease.
Insert glass stopcock into the cooling condenser and turn to the desired position.
Operation Manual Rotavapor® R-300 27/102
5 | Installation
5.5
BÜCHI Labortechnik AG
The glass stopcock performs various functions depending on its position:
Glass stopcock handle pointing right/forwards: the system is sealed.This is the standard position for distillation.
Glass stopcock handle pointing left/rearwards: system is being vented.
Glass stopcock handle pointing downwards: additional solvent can be fed into the evaporating flask via a connected backfeed tube.
Fitting PTFE stopcock (optional accessory)
28/102
Fig. 9: Cooling condenser with PTFE stopcock and backfeed tube
1 Tube on PTFE stopcock
2 Handle on three-way tap
3 Three-way tap
4 Solvent backfeed (tubing)
NOTE
The PTFE stopcock does not have to be greased.
u u u u u
Insert the tube (1) into the end of the PTFE stopcock and through the vapor duct into the evaporating flask.
Carefully insert the PTFE stopcock into the cooling condenser. When doing so, hold the PTFE stopcock so that the three-way tap (3) is still facing forwards.
NOTICE! Take care not to damage the sealing lips on the PTFE stopcock.
Rotate the PTFE stopcock 90° so that the three-way tap points upwards.
Connect the backfeed tube (4) to the PTFE stopcock.
Turn the handle on the three-way tap (2) to the desired position.
The PTFE stopcock performs various functions depending on its position:
Three-way tap handle pointing forwards: additional solvent can be fed into the evaporating flask via a connected backfeed tube.
Three-way tap handle pointing left: the system is sealed.
Three-way tap handle pointing backwards: system is being vented.
1
2
3
4
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
5.6
Installation | 5
Fitting the Interface I-300/I-300 Pro (optional accessory)
The I-300/I-300 Pro is designed for indicating, adjusting and controlling the complete distillation system. The Interface I-300 settings enable precise specification of the individual process parameters.
The interface unit can be mounted on the vertical adjustment handle.
Tools required:
Torx keys Tx20 and Tx30
1
2
3
Fig. 10: Handle of Rotavapor R-300
1 Cover
2 Communciation cable
3 Fixing screw for cover u u
Undo the fixing screw (3) on the underneath of the handle and remove the cover
(1) from the top.
Pull the communication cable (2) out of the hole in the arm of the Rotavapor
R-300.
Operation Manual Rotavapor® R-300 29/102
5 | Installation BÜCHI Labortechnik AG
1
2
3
4
5
6
Fig. 11: Fitting the holder and interface unit on the handle
1 Knurled-head screw
2 Holder for interface unit
3 Interface I-300/I-300 Pro
4 Fixing screw for holder
5 Metal plate
6 Rotavapor arm and handle u u u u u
Position the holder (2) for the interface unit on the Rotavapor arm (6). At the same time, feed the communication cable through the bottom hole in the holder.
Fix the holder to the Rotavapor arm with the screw (4) supplied. When doing so, pass the screw through the hole in the metal plate (5).
Connect the communication cable to the COM port on the rear of the interface unit.
Position the interface unit (3) on the holder. When doing so, make sure the lugs on the back of the interface unit engage in the holder.
Fix the interface unit on the holder from behind using the knurled-head screw (1) supplied. When doing so, make sure that the communication cable is not trapped.
30/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
5.7
Installation | 5
Mounting VacuBox on R-300 (optional accessory)
The VacuBox is required if the R-300 is to be operated with the Interface I-300 or
I-300 Pro.
1
2
1
1 3
Fig. 12: Mounting the VacuBox on the Rotavapor
1 Fixing screw for cover and VacuBox 3 VacuBox
2 Cover
Tools required:
Torx key Tx20 u u
Unscrew the two fixing screws (1) from the cover (2) and remove the cover.
Fit the VacuBox (3) in place of the cover using the two cover fixing screws (1) previously removed.
1
Operation Manual Rotavapor® R-300 31/102
5 | Installation
5.8
BÜCHI Labortechnik AG
Mounting LegacyBox on R-300 (optional accessory)
If legacy peripherals are to be used with the Interface I-300/I-300 Pro, a LegacyBox has to be fitted in addition to the VacuBox.
32/102
1
2
3
1
Fig. 13: Mounting LegacyBox and VacuBox on the Rotavapor
1 Fixing screws for cover
2 Cover
3 LegacyBox
4 Fixing screws for VacuBox
5 VacuBox
Tools required:
Torx key Tx20 u u
Unscrew the fixing screws (1) from the cover (2) and remove the cover.
Fit the LegacyBox (3) and VacuBox (5) together in place of the cover. To do so, use the fixing screws (4) supplied.
4
4
5
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
5.9
Installation | 5
Fitting the Woulff bottle (optional accessory)
The Woulff bottle is used to separate out particles and droplets and to equalize pressure.
The Woulff bottle can be mounted either on the inlet (vacuum) of the Vacuum Pump
V-300 (see vacuum pump manual) or on the Rotavapor® R-300.
1
2
3
Fig. 14: Mounting the Woulff bottle on the Rotavapor
1 Top part of Woulff bottle
2 Glass part of Woulff bottle
3 Holder
Precondition:
R The holder (3) for the Woulff bottle has already been fitted on the Rotavapor
R-300.
u u
Unscrew the lower, glass part (2) of Woulff bottle.
Press the top part of the Woulff bottle (1) into the holder so that it snaps into place.
u Screw the lower, glass part of the Woulff bottle into the top part again.
Operation Manual Rotavapor® R-300 33/102
5 | Installation BÜCHI Labortechnik AG
5.10
Fitting AutoDest sensor and vapor temperature sensor (optional accessory)
When using an Interface I-300/I-300 Pro there is the option of performing automatic distillation. Automatic distillation requires connection of an AutoDest sensor to the
Rotavapor R-300. The AutoDest sensor is connected to the inlet and outlet of the cooling condenser and continuously measures the following temperatures:
Temperature of the incoming coolant
Temperature of the outgoing coolant
Temperature of the vapor exiting the evaporating flask
NOTE
The AutoDest sensor has to be calibrated when first used and also when connected to a new VacuBox (see Operating Instructions I-300/I-300 Pro, Section 8.5 "Calibrating AutoDest sensor").
4
5
6
34/102
1
2
3
Fig. 15: AutoDest sensor, vapor temperature sensor and cooling condenser with evaporating flask of a
Rotavapor R-300
1 Vapor temperature sensor
2 AutoDest sensor
3 Communication connection between AutoDest sensor and VacuBox
4 Cooling condenser
5 Coolant inlet on condenser
6 Coolant outlet on condenser
NOTE
There are two arrows stamped on the AutoDest sensor indicating the direction of flow for the coolant. The hoses for the coolant must be connected according to the direction of flow as the AutoDest sensor measures the difference between the incoming and outgoing coolant temperature and communicates the readings to the VacuBox and interface unit for the purposes of automatic control.
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Installation | 5 u Connect two tubes between the AutoDest sensor (2) and the cooling condenser
(4). When doing so pay attention to the direction of flow of the coolant. The arrows on the AutoDest sensor indicate the direction of flow.
NOTE
The distance between the AutoDest sensor and the cooling condenser should not be more than 10 cm so as not to falsify the readings for the incoming and outgoing coolant temperatures in the distillation system.
u u u u
Connect a tube between the coolant inlet (5) on the AutoDest sensor and the outlet of the recirculating chiller.
Connect a tube between the coolant outlet (6) on the AutoDest sensor and either the inlet of the recirculating chiller or another cooling condenser.
Insert a vapor temperature sensor (1) in the Rotavapor R-300 and fix it in place.
Connect the outgoing cable from the AutoDest sensor to the VacuBox. Use the connection marked "VT/AS" for this lead.
NOTE
There should be no air bubbles in the coolant as otherwise correct functioning of the
AutoDest sensor is not guaranteed.
Operation Manual Rotavapor® R-300 35/102
5 | Installation BÜCHI Labortechnik AG
5.11
Fitting a foam sensor (optional accessory)
The foam sensor measures foam formation in the evaporating flask and emits a signal if the foam reaches the foam sensor. The foam is reduced by a short ventilation burst.
1 2 3 4 5 2 3 1 7
36/102
7
6
Fig. 16: Foam sensor in the evaporation unit of a Rotavapor R-300
1 Foam sensor
2 Holder for foam sensor
3 Securing nut
7 Foam sensor centrally positioned
4 Clamp screw
5 Cooling condenser
6 Evaporating flask
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Installation | 5
IMPORTANT
Risk of damage to foam sensor from contact with glass components u u
When inserting the foam sensor, make sure that the sensor rod passes centrally through the components without touching.
Use a vapor duct with a standard ground glass joint that is as large as possible
(e.g. SJ 29/32).
Precondition:
R The distillation system includes an Interface I-300/I-300 Pro and a VacuBox.
u u u u u u
Remove glass stopcock.
Fit the tapered holder (2) over the upper end of the foam sensor (1).
Slide the clamp nut (3) onto the opening for the glass stopcock.
Feed the foam sensor into the opening for the glass stopcock and through the vapor duct into the evaporating flask (6) of the Rotavapor R-300 and fix in place with the clamp nut (3). The tip of the foam sensor should be positioned approx. 4 to 5 cm below the ground neck of the evaporating flask.
Align foam sensor centrally and fix in place with the clamp screw (4).
Connect the communication cable from the foam sensor to the VacuBox. Plug the connector into the socket marked "FS".
Operation Manual Rotavapor® R-300 37/102
5 | Installation
5.12
Connecting vacuum and coolant tubing
BÜCHI Labortechnik AG
1
2
3
4
Fig. 17: Vacuum and coolant tubing connections on the cooling condenser of the R-300
1 Cooling condenser inlet
2 Connection for vapor temperature sensor
3 Cooling condenser outlet
4 Vacuum connection u u u u
Connect coolant tubes to the two coolant connections (1) and (3) using GL14 cap nuts.
Connect the vacuum tubing to the vacuum connection (4) using a GL14 cap nut.
Option 1: connect the vapor temperature sensor to connection (2) using a GL14 cap nut.
Option 2: connect the vapor temperature sensor of the AutoDest sensor to connection (2) using a GL14 cap nut. See Chapter 5.10 "Fitting AutoDest sensor and vapor temperature sensor (optional accessory)", page 34.
38/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Installation | 5
5.12.1
Overview: vacuum and coolant tubing
The following illustration provides an overall view of all vacuum and coolant tubing connections in the complete distillation system:
1
2
3
4
5
6
7
8
9
Fig. 18: Overview of tubing connections on Rotavapor R-300, Recirculating Chiller F-3xx,
Vacuum Pump V-300 and VacuBox
5 Coolant inlet on condenser 1 Connection for vapor temperature sensor
2 AutoDest sensor
3 Outlet for VacuBox connection
4 Woulff bottle outlet
6 Coolant outlet on condenser
7 Vacuum connection on Rotavapor
8 Vacuum connection on VacuBox
9 Connection for AutoDest sensor
Operation Manual Rotavapor® R-300 39/102
5 | Installation BÜCHI Labortechnik AG
5.13
Setting up the heating bath
There are two different heating bath sizes for the Rotavapor R-300:
Heating Bath B-301 for flasks up to 1 L capacity, only suitable for the use of water as heating fluid
Heating Bath B-305 for flasks up to 5 L capacity, suitable for the use of water and oil as heating medium
Whichever size of heating bath is used, it is placed on the Heating Bath B-300 Base.
Depending on which size of heating bath is used, the heating bath base has to be pushed in a different amount on the Rotavapor rail. With the smaller heating bath, the
B-301, the base is pushed in as far as it will go. With the larger heating bath, the
B-305, the heating bath base must not be pushed all the way in as otherwise the
Rotavapor lift will not be able to lower. A mechanical catch on the Heating Bath B-305 makes sure that the heating bath base is not pushed in too far.
40/102
1
2
Fig. 19: Heating Bath B-305 and Heating Bath B-300 Base
1 Heating Bath B-305 2 Heating Bath B-300 Base
WARNING
Risk of burns if Heating Bath B-301 is used incorrectly u Do not use oil as heating fluid in the Heating Bath B-301.
IMPORTANT
Risk of heating bath corrosion due to use of unsuitable heating fluid u If pure distilled or de-ionised water is used, add approx. 1 g of Borax (Na
2
B
4
O
7
x
10 H
2
O) per liter of water.
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Installation | 5
The recommended fluid for use in the heating bath is water. Normal tap water may be mixed with distilled water with a mixing ratio of up to 1:1 according to the water hardness.
u u u u
Slide the Heating Bath B-300 Base (2) onto the base of the Rotavapor R-300.
Make sure that there are no objects in the Rotavapor base recess as this is where the data is transferred from the heating bath base to the Rotavapor by infra-red signals.
Place the heating bath (1) centrally on the base.
Fill the heating bath with suitable fluid.
5.14
Fitting the protection shield (optional)
The protection shield protects against solvent splashes, hot heating fluid splashes and glass splinters in the event of implosions.
NOTE
The protection shield only protects against splashes to the front. Protection against splashes in other directions must be provided by the user.
1
2
Fig. 20: Fitting the protection shield on the Rotavapor
1 Screw holes 2 Button on handle u Insert the studs on the protection shield mounting bracket into the screw holes (1) on the Rotavapor drive unit.
Operation Manual Rotavapor® R-300 41/102
5 | Installation BÜCHI Labortechnik AG u u
Secure the protection shield by inserting the pin supplied in the hole for the mounting bracket.
Adjust the position of the protection shield to the desired angle by pressing the button on the handle (2).
5.15
Connecting the Rotavapor to the power supply
The Rotavapor and the heating bath each have their own separate power supply connection.
Rotavapor
42/102
1
Fig. 21: Power supply connection on Rotavapor R-300
1 Power supply connection
NOTE
When connecting the Rotavapor and the heating bath to the power supply, it is important to ensure that they are grounded. The use of 3-core power cables and
3-pin plugs will ensure that is the case.
u u
Make sure that the available power supply matches the rating indicated on the type plate.
Plug the power cord into the socket (1) on the Rotavapor and then into a mains power socket.
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Installation | 5 u If an extension lead is required, make sure that it is grounded and has a suitable power rating.
Heating bath base
1
2
Fig. 22: Power supply connection on heating bath base
1 Fuse rating plate 2 Power supply connection u Plug a separate power cord into the socket (2) on the heating bath base and then into a mains power socket.
Operation Manual Rotavapor® R-300 43/102
5 | Installation BÜCHI Labortechnik AG
5.16
Assembling the BUCHI distillation system
In order to use the Rotavapor® R-300 to best effect, we recommend that it is used together with the following equipment:
44/102
Fig. 23: Interface unit, VacuBox, Rotavapor, vacuum pump and recirculating chiller
1 Recirculating Chiller F-3xx
2 Rotavapor R-300 with heating bath
B-305
3 VacuBox
4 Vacuum Pump V-300
5 Interface I-300/I-300 Pro
The F-3xx is a recirculating chiller with a sealed circulation system. It is available in various capacity ratings.
The Interface I-300/I-300 Pro together with the VacuBox can be used to control and monitor the vacuum. It can control the Rotavapor, the Vacuum Pump V-300 and the
Recirculating Chiller F-3xx and maintain a set constant pressure.
The Vacuum Pump V-300 is a diaphragm pump designed for evacuating laboratory apparatus. It can be operated either as a standalone device or combined with optional accessories such as an interface unit and a secondary cold trap to form a complete vacuum system. The laboratory equipment to be evacuated is connected to the vacuum pump and the VacuBox by means of vacuum tubing. See Overview: setting up vacuum tubing connections
Data communication between the laboratory equipment takes place via the communication ports. See Chapter 5.16.2 "Connecting communication cables to the
Rotavapor", page 46.
The coolant circulates around the distillation system through a separate circulation system. See Overview: setting up coolant tubing connections.
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Installation | 5
5.16.1
Overview: setting up communication connections
The laboratory apparatus can be connected in any order. Important: as well as the
Interface I-300/I-300 Pro, a VacuBox also has to be connected.
Below is an example of the connections between the laboratory apparatus.
Vacu
Box
Vacuum Pump
V-300 / V-600
Recirculating
Chiller F-3XX
Rotavapor
R-300
Interface I-300/
I-300 Pro
Fig. 24: Schematic diagram of communication connections between the BUCHI laboratory equipment (example) u u u u
Connect the Recirculating Chiller F-3xx to the Rotavapor R-300.
Connect the Rotavapor R-300 to the VacuBox.
Connect the VacuBox to the Vacuum Pump V-300/V-600.
Connect Rotavapor to the Interface I-300/I-300 Pro.
Operation Manual Rotavapor® R-300 45/102
5 | Installation BÜCHI Labortechnik AG
5.16.2
Connecting communication cables to the Rotavapor
The connections between the BUCHI laboratory apparatus are established by means of a standard BUCHI communication cable (COM) in each case.
2
Fig. 25: Communication cable connections on Rotavapor
1 Sensor connection, not used 2 Standard BUCHI communication ports (COM) u u
Plug the communication cable for connection to other BUCHI laboratory equipment into one of the standard BUCHI communication ports (2).
Plug the communication cable into the green communication port on the other item of laboratory equipment.
46/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Installation | 5
5.16.3
Overview: setting up coolant tubing connections
The tubing connections between the various items of BUCHI laboratory equipment form a sealed circulation system. The starting and finishing point is always the recirculating chiller (F-3xx).
Below is an example of the tubing connections between the laboratory apparatus.
1
Recirculating
Chiller F-3XX
2
3 4
5
6
Vacuum Pump
V-300 / V-600
Rotavapor
R-300
Fig. 26: Coolant tubing connections in a BUCHI distillation system (example)
1 Inlet on Recirculating Chiller F-3xx 4 Condenser outlet on Rotavapor
R-300
2 Outlet on Recirculating Chiller F-3xx 5 secondary cold trap inlet on Vacuum
Pump V-300
3 Condenser inlet on Rotavapor R-300 6 Secondary cold trap outlet on Vacuum Pump V-300 u u u
Connect a tube between the outlet of the recirculating chiller (2) and the inlet of the condenser on the Rotavapor R-300 (3).
Connect a tube between the outlet of the condenser on the Rotavapor R-300 (4) and the inlet of the secondary cold trap on the Vacuum Pump V-300 (5).
Connect a tube between the outlet of the secondary cold trap on the Vacuum
Pump V-300 (6) and the inlet of the recirculating chiller (1).
NOTE
Use GL14 hose barbs for the tubing connections.
Secure tubes with spring clips where necessary.
NOTE
The R-300 is also suitable for use with water coolant.
Operation Manual Rotavapor® R-300 47/102
5 | Installation BÜCHI Labortechnik AG
5.16.4
Overview: setting up vacuum tubing connections
The vacuum tubing connections in a typical BUCHI distillation system lead from the
Rotavapor R-300 via a Woulff bottle to the Vacuum Pump V-300. The vacuum is measured by means of the VacuBox, which is also connected to the Woulff bottle.
Rotavapor
R-300
3
Vacuum Pump
V-300 / V-600
2
1
4 5 6
Vacu
Box
Extraction device
Fig. 27: Coolant tubing connections in a BUCHI distillation system
1 Secondary cold trap outlet
2 Vacuum pump outlet
3 Vacuum pump inlet
4 Woulff bottle outlet (PUMP)
5 Woulff bottle inlet (CONTR)
6 VacuBox valve connection u u u u
Connect a tube between the Rotavapor R-300 and the top inlet of the Woulff bottle.
Connect a tube between the outlet of the Woulff bottle marked PUMP (4) and the pump inlet (3).
Connect the secondary cold trap to the pump outlet (2).
For measuring and controlling the vacuum, connect a tube between the inlet of the
Woulff bottle marked CONTR (5) and the VacuBox (6).
The pressure is measured in the VacuBox. The current working pressure can be indicated and controlled by means of the Interface I-300/I-300 Pro.
NOTE
The VacuBox and Woulff bottle can be mounted either on the Rotavapor R-300 or the Vacuum Pump V-300. What is important is that the VacuBox and Woulff bottle are as close as possible to each other (on the same device) as otherwise there is a vacuum control lag.
48/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
5.17
Basic settings
1
2
3 on Lift set max.95°
Set
46
°C
50
°C STOP
Installation | 5
Fig. 28: Heating bath basic settings
1 Maximum temperature
2 Actual temperature
3 Set temperature
Setting the maximum temperature
NOTE
Maximum possible temperature settings (1) are defined for the heating bath: The
Heating Bath B-305 can be set to a maximum temperature of 95 °C, 180 °C or 220
°C, depending on which fluid is in the bath. The Heating Bath B-301 can be set to a maximum temperature of 95 °C. For safety reasons, the lowest possible maximum temperature should be chosen.
u To set the maximum temperature, press and hold the control knob (6).
The Settings menu appears, identifiable by the gear symbol on the display.
u Turn the control knob to select the desired maximum temperature, and press it briefly to confirm the selection.
Locking the set temperature
The heating bath has a locking function that prevents the set temperature being inadvertently altered.
u u
To lock the set temperature, press and hold the control knob (6) until the padlock symbol (4) appears on the display.
Press the control knob again to confirm.
The Settings menu appears, identifiable by the gear symbol on the display.
u To cancel the lock function, press and hold the control knob again until the padlock symbol disappears.
4 Set temperature locked
5 START/STOP function activated on pressing navigation control
6 Control knob for setting the required temperature and starting/stopping the heating process
4
5
6
Operation Manual Rotavapor® R-300 49/102
5 | Installation BÜCHI Labortechnik AG
5.18
Quick check
u u u u u
To complete the installation process, switch on the device at the master switch and check the following points:
Switch on the rotary drive unit, change the rotation speed and check that the evaporating flask rotates at a different speed.
CAUTION! Risk of skin burns! Make sure that the heating bath is filled, switch on the heating bath and check that the heating fluid heats up. See Chapter 6.1.1
"Preparing the heating bath", page 51.
Check that the height of the rotary drive unit can be adjusted. See Chapter 6.1.5
"Raising and lowering rotary drive unit", page 55.
Check system for leaks, see Chapter 7.2 "Checking the system for leaks", page 68.
50/102 Operation Manual Rotavapor® R-300
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6 Operation
6.1
6.1.1
Operation | 6
Preparations
Preparing the heating bath
CAUTION
Risk of skin burns from hot fluids and surfaces u u u u
Do not put your hands in the hot fluid.
Do not carry, shift, tip or otherwise move the heating bath when it is filled with hot fluid.
Do not fill the heating bath right to the very top. Allow for the expansion of the fluid when heated.
Do not switch on the heating bath when it is empty.
CAUTION
Using oil as a heating fluid
Risk of skin burns from oil splashes u u
Never pour water into hot oil.
Make sure that the oil used is suitable for these purposes and the desired temperatures.
1 on Lift set max.95°
Set
46
°C
50
°C STOP
3
4
9
5
Fig. 29: Heating bath display
1 Maximum temperature
2 "Lift set" indicates that a lower limit has been set for the Rotavapor lift.
3 Actual temperature
4 Set temperature
6 Set temperature locked
7 Connection symbol – heating bath is being controlled by an Interface I-300/
I-300 Pro
8 START/STOP function activated on pressing navigation control
9 Control knob for setting the required temperature and starting/stopping the heating process
5 ON/OFF master switch
6
7
8
Operation Manual Rotavapor® R-300 51/102
6 | Operation
6.1.2
BÜCHI Labortechnik AG u Switch on the device at the master switch (5).
The heating bath temperature (4) last set is displayed.
u u
Set the maximum temperature (1), see Chapter 5.17 "Basic settings", page 49.
Set the desired temperature using the control knob (9).
The current actual temperature (3) and the specified temperature (4) are shown on the display.
u Lock the set temperature, see Chapter 5.17 "Basic settings", page 49.
Fitting the evaporating flask
IMPORTANT
Risk of evaporating flask damage if fitted incorrectly u u
When fitting the evaporating flask make sure that the edge of the glass does not strike the vapor duct.
Tighten combi-clip no more than hand-tight.
1
52/102
Fig. 30: Fitting the evaporating flask
1 Combi-clip
2 Vapor duct
3 Evaporating flask u u
Carefully fit evaporating flask (3) onto the vapor duct (2).
Screw combi-clip (1) clockwise until hand-tight.
Operation Manual Rotavapor® R-300
2
3
BÜCHI Labortechnik AG
6.1.3
Operation | 6
Adjusting immersion angle of evaporating flask
The immersion angle of the evaporating flask has to be adjusted according to the size and capacity of the heating bath (B-301 or B-305) and the evaporating flask.
1
2
Fig. 31: Adjusting the immersion angle
1 Cooling condenser 2 Adjuster button for immersion angle
Precondition:
R Rotavapor is not in operation.
u u
Hold the cooling condenser (1) firmly with one hand and press and hold the adjuster button (2) with the other hand.
Adjust the immersion angle.
NOTE
When the Rotavapor lift is in its lowered position, there must be at least 10 mm clearance between the edge of the heating bath and the evaporating flask.
u u
Release the adjuster button to lock the rotary drive unit in position again.
Check the vertical travel limit for the lift and, if necessary, readjust the immersion angle or the end stop, see Chapter 6.1.5 "Raising and lowering rotary drive unit", page 55.
Operation Manual Rotavapor® R-300 53/102
6 | Operation
6.1.4
Fitting the receiving flask
BÜCHI Labortechnik AG
1
2
Fig. 32: Fitting the receiving flask
1 Ball joint clamp 2 Receiving flask u u
Fit the receiving flask (2) onto the condenser from below, hold it firmly in place and secure it with the ball joint clamp (1).
If the connection is not sufficiently airtight, apply a thin coat of Glisseal 40 red laboratory grease to the ground glass joint.
54/102 Operation Manual Rotavapor® R-300
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6.1.5
Operation | 6
Raising and lowering rotary drive unit
The rotary drive unit together with the glass components can be raised or lowered either manually or by motor power, depending on the version of the R-300. To prevent the evaporating flask fouling on the heating bath, a minimum depth stop can be set.
CAUTION
Risk of scalding if heating bath overflows u u
When immersing the evaporating flask, make sure that the fluid does not overflow due to the displacement.
When the evaporating flask is rotating look out for splashing fluid.
CAUTION
Risk of burns from splashing heating fluid u u
When the evaporating flask is rotating look out for splashing fluid.
Use the protection shield and wear protective clothing.
CAUTION
Risk of injury when adjusting apparatus height u u
Make sure that your fingers are not trapped when adjusting the apparatus height, especially when using the safety guard.
Make sure that all tubing is long enough and is not under strain after making the adjustment.
IMPORTANT
Risk of evaporating flask damage due to collision with edge of heating bath u Make sure that there is at least 10 mm clearance between the evaporating flask and the edge and/or bottom of the heating bath.
Operation Manual Rotavapor® R-300 55/102
6 | Operation BÜCHI Labortechnik AG
Fig. 33: Clearance between evaporating flask and edge of heating bath
Electrical height adjustment
1
2
56/102
Fig. 34: Rotavapor arm
1 Set button for adjusting the depth stop
2 Handle on Rotavapor arm u u
To raise or lower the rotary drive unit, tip the handle (2) up or down to obtain the desired position.
To set a depth stop, move to the drive unit to the desired height and press and hold the Set button (1) for approx. 2 seconds.
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
3
Operation | 6 on Lift set max.95°
Set
46
°C
50
°C STOP
Fig. 35: Heating bath display
3 "Lift set" indication for depth stop u
The display of the heating bath base shows "Lift set" (3).
To delete a depth stop, press and hold the Set button (1) for at least three seconds until "Lift set" disappears from the display.
The position of the rotary drive unit is indicated on the display of the Heating Bath
B-300 Base and the Interface I-300/I-300 Pro as follows:
If no depth stop has been set, the distance of the lift from the top end is indicated, starting from 0 mm as the highest position. Any position below that is indicated accordingly by a negative figure.
If a depth stop has been set, the distance of the lift from the bottom end is indicated, starting from 0 mm as the lowest position. Any position above that is indicated accordingly by a positive figure.
NOTE
2 different speeds: the lift moves down quickly until it is 2 cm from the depth stop; it then moves slowly over the last 2 cm to the depth stop.
Operation Manual Rotavapor® R-300 57/102
6 | Operation
Manual height adjustment
BÜCHI Labortechnik AG
1
2
Fig. 36: Rear view of Rotavapor
1 Handle on Rotavapor arm 2 Stop screw u u
To raise or lower the rotary drive unit, tip the handle (1) up or down and move the rotary drive unit to the desired position.
To set a depth stop, press the Set button.
5 The stop screw (2) drops down onto the base of the Rotavapor. That is the mechanical depth stop.
58/102 Operation Manual Rotavapor® R-300
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6.2
Operation | 6
Performing distillation
DANGER
Risk of poisoning from inhalation of hazardous vapors u u u u u u
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 replace them if necessary.
Do not distill any unknown fluids.
Observe the safety data sheets for all fluids used.
DANGER
Explosion risk from distillation of hazardous materials u u u u u
Do not distill solvents that produce explosive mixtures of gases.
Make sure that there is always a sluggishly reactive atmosphere inside the system.
Discharge any electrostatic charge by suitable grounding arrangements.
Keep sources of ignition away from the apparatus.
Use the protection shield and fume extractor, and wear protective clothing.
WARNING
Risk of explosion from excessive internal pressure
The evaporating flask and/or the condenser could explode if the internal pressure produced by evaporation becomes too great.
u Make sure that the pressure in the system is never greater than atmospheric pressure.
CAUTION
Risk of skin burns from hot components u Do not touch hot components unless wearing suitable protective gloves.
CAUTION
Risk of injury from solvent splashes and hot heating fluid splashes u u u
Use the protection shield.
Make sure that protection against splashes in all directions is provided.
When the evaporating flask is rotating look out for splashing fluid.
Operation Manual Rotavapor® R-300 59/102
6 | Operation
6.2.1
Operating the Rotavapor without control system (interface)
BÜCHI Labortechnik AG
1
60/102
2
Fig. 37: Components for manual control of Rotavapor R-300
1 Control knob on rotary drive unit 2 Control knob on heating bath
NOTE
When controlling the Rotavapor R-300 manually, it is important to adjust and switch on the laboratory equipment involved in the correct order.
To achieve optimum distillation results, the following procedure is recommended: u u u u u u u
Prepare the heating bath, see Chapter 6.1.1 "Preparing the heating bath", page 51, and start the heating process by briefly pressing the control knob on the heating bath (2).
Switch on the cooling system. Set the coolant temperature (max. 20 °C) or the flow rate (at least 40 L/h).
Switch on the Rotavapor at the master switch.
Fit the filled evaporating flask and the receiving flask.
Close the glass stopcock.
Press the control knob on the rotary drive unit (1) and start rotation at a slow speed. The rotation speed can be adjusted by means of the control knob.
Switch on the vacuum pump and, if necessary, set the required pressure. The boiling point of the solvent must be 20 °C below the temperature of the heating bath.
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
6.2.2
Operation | 6 u u u u u Lower the rotating evaporating flask into the heating bath. CAUTION! Risk of pinching injuries!
If using the protection shield, make sure that your fingers or other parts of the body are not trapped.
Immerse the evaporating flask in the heating bath.
Increase rotation to the desired speed.
Wait 1 – 2 minutes to make sure distillation starts.
If necessary, adjust the vacuum and/or the heater temperature see Chapter 6.2.4
"Optimization distillation", page 62.
Operating Rotavapor with Interface I-300/I-300 Pro
The Rotavapor and the entire distillation system can be fully controlled by an Interface
I-300/I-300 Pro. The Interface I-300/I-300 Pro settings enable precise specification of the individual process parameters. For example:
Rotation speed of the evaporating flask
Specified temperature of the heating bath
Specified temperature of the coolant
Vacuum level
Duration of the distillation process
1
2
3
2
4
ST
OP
Fig. 38: Front view of Interface I-300 showing controls
1 Display
2 Function buttons
3 STOP button (emergency stop)
4 Navigation control u Connect the Interface I-300/I-300 Pro and the VacuBox, see Chapter 5.16.1
"Overview: setting up communication connections", page 45 and the relevant chapters in the operating instructions of the I-300/I-300 Pro.
NOTE
To save energy, the Interface I-300/I-300 Pro offers an "eco mode" option which can be activated if the distillation system is inactive. In eco mode, the distillation system shuts down the activity of the heating bath after a defined delay period. The heating bath does not reheat until the heating bath temperature has dropped to a defined minimum temperature. For details, refer to the operating instructions of the Interface
I-300/I-300 Pro.
Operation Manual Rotavapor® R-300 61/102
6 | Operation
6.2.3
BÜCHI Labortechnik AG
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. To achieve that, the following settings are recommended:
20 °C
∆ 20 °C
62/102
6.2.4
40 °C 2
∆ 20 °C
60 °C 3
Fig. 39: Distillation conditions
1 Coolant temperature: 20 °C
2 Vapor temperature: 40 °C
3 Heating bath temperature: 60 °C
The temperature difference between heating bath and evaporating flask and between evaporating flask and cooling condenser should be 20 °C in each case.
The pressure in the evaporating flask should be set so that the boiling point of the solvent is around 40 °C. See Chapter 10.1 "Solvent table", page 77.
The flow rate of the coolant depends on the type of coolant used and the pump capacity of the cooler but should be at least 40 to 50 L/h.
Those settings offer the following advantages:
The evaporating flask can be replaced without the risk of skin burns.
The evaporation rate of the water in the heating bath is low.
The energy of the heating bath is efficiently utilized.
Optimization distillation
Depending on the solvent involved, it may also be possible to further optimize the distillation process. The distillation should always be set up so that the condensate does not cover more than three quarters of the coil in the cooling condenser. There should be no condensate visible in the top quarter.
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
1
Operation | 6
¾
Fig. 40: Cooling condenser
1 Cleaning hole
WARNING
Risk of explosion from excessive internal pressure
The evaporating flask and/or the condenser could explode if the internal pressure produced by evaporation becomes too great.
u Make sure that the pressure in the system is never greater than atmospheric pressure.
NOTE
The stopcock should only be inserted in the cooling condenser, not secured. If an abrupt rise in pressure occurs during distillation, the stopcock will then be able to pop out, which is intended. That guarantees that the system pressure is never greater than atmospheric pressure.
NOTE
If a distillation process is to be carried out at normal pressure, the glass components
– for example the cleaning hole (1) on the cooling condenser – should be opened to prevent pressure build-up.
If the condensation is below 3/4 of the condenser: u Increase the vacuum.
That will lower the boiling point and more vapor will enter the condenser.
u In applications where no vacuum is applied, raise the temperature of the heating bath if necessary.
That will cause more solvent to evaporate.
Operation Manual Rotavapor® R-300 63/102
6 | Operation
6.2.5
BÜCHI Labortechnik AG
If the condensation is above 3/4 of the condenser: u Decrease the vacuum.
That will raise the boiling point and less vapor will enter the condenser.
u In applications where no vacuum is applied, lower the temperature of the heating bath.
That will cause less solvent to evaporate.
Adding solvent during distillation
Precondition:
R A vacuum pump is connected and running.
R A backfeed tube leading from the glass stopcock to the evaporating flask is fitted.
1
2
Fig. 41: Cooling condenser with glass stopcock and backfeed tube
1 Glass stopcock 2 Backfeed tube u u
Connect a backfeed tube (2) for the solvent to the glass stopcock (1) and hold it in the solvent.
Turn the glass stopcock until the handle is pointing downwards.
Solvent is drawn into the evaporating flask by the vacuum.
u u u
Make sure that there is not more than 3 kg of solvent in the evaporating flask and that the evaporating flask is not overfilled.
Make sure that there is sufficient space for the condensate in the receiving flask.
Close the glass stopcock.
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6.3
6.3.1
Operation | 6 u u u u
Finishing distillation
u u u u u u u
Slow down the rotation speed or reduce it to a minimum.
Raise the rotary drive unit (see Chapter 6.1.5 "Raising and lowering rotary drive unit", page 55). CAUTION! Risk of burns from hot heating fluid splashes.
When the evaporating flask is rotating look out for splashing fluid.
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 temperature of the evaporating flask and, if necessary, allow it to cool down or else wear suitable protective gloves.
Remove the evaporating flask, see Chapter 6.3.1 "Removing the evaporating flask", page 65.
Turn off the coolant supply.
Remove the receiving flask, see Chapter 6.3.2 "Removing the receiving flask", page 66.
Dry the Rotavapor, see Chapter 7.8 "Removing solvent accumulations", page 71.
Clean the Rotavapor and all glass components, see Chapter 7 "Cleaning and servicing", page 67.
Removing the evaporating flask
2
Fig. 42: Evaporating flask on Rotavapor R-300
1 Combi-clip
2 Evaporating flask
3 Locking button u u u u u u u
Slow down the rotation speed or reduce it to a minimum.
Raise the rotary drive unit (see Chapter 6.1.5 "Raising and lowering rotary drive unit", page 55).
Vent the Rotavapor.
Turn off the rotary drive unit (set the rotation speed to 0 rpm).
CAUTION! Risk of skin burns from hot evaporating flask . Check the temperature of the evaporating flask and, if necessary, allow it to cool down or else wear suitable protective gloves.
Firmly hold the evaporating flask (2) and release the combi-clip (1) by screwing it counter-clockwise.
Detach the evaporating flask.
Operation Manual Rotavapor® R-300 65/102
6 | Operation
6.3.2
BÜCHI Labortechnik AG u If the evaporating flask sticks because of chemical residues, press the lock release button (3) and twist the combi-clip counter-clockwise to allow the flask to be removed.
Removing the receiving flask
1
2
Fig. 43: Receiving flask on Rotavapor R-300
1 Ball joint clamp 2 Receiving flask u u u u u u
Slow down the rotation speed or reduce it to a minimum.
Raise the rotary drive unit (see Chapter 6.1.5 "Raising and lowering rotary drive unit", page 55).
Vent the Rotavapor.
Turn off the rotary drive unit (set the rotation speed to 0 rpm).
Firmly hold the receiving flask (2), remove the ball joint clamp (1) and remove the receiving flask.
Make sure that any dripping condensate cannot cause any damage.
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7
Cleaning and servicing | 7
Cleaning and servicing
NOTE
Users may only carry out the servicing and cleaning operations described in this section.
Any servicing and repair work which involves opening up the housing may only be carried out by BUCHI service technicians.
u u
Use only genuine BUCHI consumables and spare parts in order to ensure correct operation of the device and preserve the warranty.
Before carrying out any servicing work, empty the heating bath and all glass components.
7.1
Inspecting and cleaning the vapor duct
1
Fig. 44: Vapor duct on Rotavapor R-300
1 Flange nut
2 Locking button
3 Combi-clip u u u u u u u u u
Switch off the device.
Remove the evaporating flask, see Chapter 6.3.1 "Removing the evaporating flask", page 65.
Remove the receiving flask, see Chapter 6.3.2 "Removing the receiving flask", page 66.
Remove the cooling condenser from the rotary drive unit. To do so, hold the cooling condenser firmly with one hand and unscrew the flange nut (1) with the other hand.
Press and hold the lock release button (2) on the front of the rotary drive unit.
Turn the combi-clip (3) clockwise until the vapor duct is released.
Remove the vapor duct and visually inspect it for damage, wear marks and residues.
Clean the vapor duct with a paper towel and water or ethanol.
Refit the vapor duct and cooling condenser, see Chapter 5.3 "Fitting the vapor duct, vacuum gasket and cooling condenser", page 26.
Operation Manual Rotavapor® R-300 67/102
7 | Cleaning and servicing
7.2
BÜCHI Labortechnik AG
Checking the system for leaks
Recommendation:
When using an Interface I-300/I-300 Pro there is the option of performing a leak test to check the system for leaks. For details, refer to the operating instructions of the
Interface I-300/I-300 Pro.
Precondition:
R A vacuum pump with a pressure gauge is connected.
R The system is dry.
u u u u u
Make sure that the system is dry. Remove any solvent accumulations if necessary.
Make sure that all flasks are fitted and the glass stopcock is closed.
Connect the vacuum pump and evacuate the R-300 to a pressure of 50 mbar.
Switch off the vacuum pump. If necessary, disconnect the vacuum tubing so as to exclude the vacuum pump as a possible source of a leak.
Check the pressure after one minute.
5 If the pressure has risen by less than 5 mbar after one minute, the system is air-tight.
If the system is not air-tight: u u u
Check all seals, see Chapter 7.4 "Checking seals", page 70.
Examine all tubing and replace if they are brittle or cracked.
Grease ground glass joints if necessary.
NOTE
Damaged ground glass joints can also lead to leaks in the system.
68/102 Operation Manual Rotavapor® R-300
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7.3
Fitting GL14 union nut with tube seal
1
2
3
Cleaning and servicing | 7
Fig. 45: Fitting GL14 union nut with tube seal (example shows VacuBox)
1 Tube seal
2 GL14 union nut
3 Tubing u u u u
Insert the tube seal (1) in the GL14 union nut (2) ensuring it is straight. NO-
TICE! Risk of damaging tube seal. Make sure that the tube seal does not twist or jam in the GL14 union nut.
Loosely screw the GL14 union nut together with tube seal onto the device concerned (example shows VacuBox) or the Woulff bottle.
Carefully insert the end of the tube (3) into the GL14 union nut and tube seal.
Tighten the GL14 union nut and tube seal.
Operation Manual Rotavapor® R-300 69/102
7 | Cleaning and servicing
7.4
BÜCHI Labortechnik AG
Checking seals
Seals are wearing parts. They have to be regularly inspected, cleaned and, if necessary, replaced. The life of a seal depends on how much it is used and how well it is looked after.
4
1
2
5
6
7
3
Fig. 46: Seals on Rotavapor and cooling condenser
1 Coolant seal
2 Vacuum seal
3 Sensor seal
4 Cleaning hole seal
5 Coolant seal
6 Feed tubing seal
7 Vacuum connection seal u u u
Remove seals and inspect for damage and cracks.
Rinse intact seals in water or ethanol and dry with a soft cloth.
Replace damaged seals and check the corresponding glass contact faces for damage (e.g. wear marks).
NOTE
New PTFE seals require approx. 10 hours to achieve an optimum seal.
70/102 Operation Manual Rotavapor® R-300
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7.5
Cleaning and servicing | 7
Cleaning the cooling condenser
u u u
Using a wash bottle, squirt ethanol into the cleaning hole of the cooling condenser and rinse it out.
After rinsing allow the ethanol to drain out.
Use an alkaline cleaning agent to remove stubborn dirt (e.g. algae in the condenser coil).
7.6
Cleaning the heating bath
IMPORTANT
Risk of short circuit from fluid penetration into device u u
Do not immerse heating bath or rotary drive unit in water or pour water over them.
Only wipe down the casing with a damp cloth.
7.7
7.8
The inside of the heating bath bowl should be cleaned regularly and at the latest if:
the heating bath is contaminated
limescale deposits start to form
the steel surface of the heating bath starts to rust u u u u
Unplug the power supply for the heating bath and rotary drive unit.
Allow the heating bath to cool down then empty it.
Remove small amounts of limescale in the bowl of the heating bath using non-abrasive cleaners (e.g. household cleaner and washing-up sponge).
Use acetic acid to dissolve stubborn limescale deposits. Afterwards thoroughly rinse out the bath.
u u u
Cleaning the Woulff bottle
Unscrew the glass part of the Woulff bottle from the holder.
Clean the glass part with ethanol to remove residues.
Screw the glass part back into the holder.
Removing solvent accumulations
Before any extended period in which the device is not used (e.g. overnight) all fluids must be removed from the device and the system dried.
u u u u u u Fit a clean and dry evaporating flask and receiving flask. See Chapter 6.1.2
"Fitting the evaporating flask", page 52 and Chapter 6.1.4 "Fitting the receiving flask", page 54.
Make sure that the glass stopcock is closed.
Connect the vacuum pump and evacuate the Rotavapor as much as possible.
Allow the vacuum pump to run for at least 2 to 3 minutes.
Vent the Rotavapor.
Check that all solvent accumulations have been removed.
Operation Manual Rotavapor® R-300 71/102
8 | Help with faults
8
8.1
BÜCHI Labortechnik AG
Help with faults
Faults, possible causes and remedies
Fault
Device does not work
Possible cause
Device is not connected to power supply
Fuse blown
Heating bath fails to heat up
Device is not connected to power supply
High temperature cut-out has tripped u Check power supply (see
Chapter 5.15 "Connecting the Rotavapor to the power supply", page 42).
u Reset the overheat safety cut-out (see Chapter 8.2.1
"Resetting overheat safety cut-out on heating bath", page 74).
Fuse blown u u
Replace fuse (see
Chapter 8.2.2 "Replacing fuse in heating bath base", page 75).
If fault recurs, contact
BUCHI Customer Service.
System leaking Ground glass joints not greased u Grease ground glass joints.
Tubing leaking
Remedy u Check power supply (see
Chapter 5.15 "Connecting the Rotavapor to the power supply", page 42).
u u
Replace fuse (see
Chapter 8.2.2 "Replacing fuse in heating bath base", page 75).
If fault recurs, contact
BUCHI Customer Service.
Electric lift does not operate
Seal defective
Heating Bath B-300 Base and heating bath positioned too far to the left.
u Replace tubing (see
Chapter 5.12 "Connecting vacuum and coolant tubing", page 38).
u Replace seal (see
Chapter 7.4 "Checking seals", page 70).
u Move Heating Bath B-300
Base to the right until it snaps into position.
72/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Help with faults | 8
Fault
Vacuum is not achieved
Optimum distillation not achieved
Possible cause
Back-evaporation from the receiving flask
Temperature difference between vapor and coolant less than 20 °C
System leaking
If using a glass filter pump: water pressure of glass filter pump too low
Vacuum pump too weak
Too much back-evaporation from the receiving flask (especially with solvent mixtures)
Other faults in distillation process (e.g. sudden cooling, too little heat flow, etc.)
Remedy u Empty the receiving flask
(see Chapter 6.3.2
"Removing the receiving flask", page 66).
u Increase cooling (see
Chapter 6.2.3 "Adjusting distillation conditions", page 62).
u Check system for leaks (see
Chapter 7.2 "Checking the system for leaks", page 68).
u Increase water flow (see pump operating instructions).
u Use suitably dimensioned vacuum pump.
u Empty receiving flask and restart distillation (see
Chapter 6.3.2 "Removing the receiving flask", page 66, Chapter 6.1.4
"Fitting the receiving flask", page 54 and Chapter 6.2
"Performing distillation", page 59).
u u
Check temperatures of heating bath and coolant and adjust as necessary
(see Chapter 6.1.1
"Preparing the heating bath", page 51 and/or cooler operating instructions).
Lower pressure until distillation resumes (see vacuum pump operating instructions).
Operation Manual Rotavapor® R-300 73/102
8 | Help with faults
8.2
8.2.1
BÜCHI Labortechnik AG
Resetting safety functions
Resetting overheat safety cut-out on heating bath
The overheat safety cut-out trips if oil is used in the Heating Bath B-301 or the temperature control fails. In that case, the power supply for the heating bath is switched off. If the wrong heating fluid has been used for the Heating Bath B-301, the overheat safety cut-out can be reset.
The overheat safety cut-out is on the underneath of the heating bath.
CAUTION
Risk of skin burns from hot components u Do not touch hot components unless wearing suitable protective gloves.
2
Fig. 47: Undersides of Heating Baths B-301 and B-305
1 Overheat safety cut-out on B-305 2 Overheat safety cut-out on B-301 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 red pin (1)/(2) on the underside of the heating bath.
5 The overheat safety cut-out is reset.
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BÜCHI Labortechnik AG
8.2.2
Replacing fuse in heating bath base
The fuse is on the rear of the heating bath base.
Help with faults | 8
1
2
Fig. 48: Fuse in heating bath base
1 Fuse rating plate 2 Fuse holder u u u u u u u u
Allow the heating bath to cool down then lift it carefully off the base.
Slide the base to the right off the base of the Rotavapor.
Disconnect the power cord.
Open the fuse holder (2) with a large screwdriver.
Replace the blown fuse with an intact one of the same rating.
Screw the fuse holder (2) back in.
Reconnect the power cord.
Slide the base back onto the Rotavapor® base from the right.
NOTE
The fuse must match the specifications on the fuse rating plate.
Operation Manual Rotavapor® R-300 75/102
9 | Taking out of service and disposal
9 Taking out of service and disposal
9.1
9.2
BÜCHI Labortechnik AG u u u
Taking out of service
u Remove all fluids from the glass components (see Chapter 7.8 "Removing solvent accumulations", page 71).
Switch off the device.
Unplug the power supply for the heating bath and rotary drive unit.
Remove all glass components.
Disposal
The operator is responsible for proper disposal of the Rotavapor®.
u When disposing of equipment observe the local regulations and statutory requirements regarding waste disposal.
76/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
10 Appendix
Appendix | 10
Solvent
10.1
Solvent table
Formula
Acetone n -pentanol
Benzene n -butanol tertbutanol
Chlorobenzene
Chloroform
Cyclohexane
CH
3
H
6
O
C
5
H
12
O
C
6
H
6
C
4
H
10
O
C
4
H
10
O
C
6
H
5
Cl
CHCl
3
C
6
H
12
Diethyl ether C
4
H
10
O
1,2-dichloroethane C
2
H
4
Cl
2 cis -1,2dichloroethene
C
2
H
2
Cl
2
C
2
H
2
Cl
2 trans -1,2dichloroethene
Di-isopropyl ether
Dioxane
DMF (dimethylformamide)
C
6
H
14
O
C
4
H
8
O
2
C
3
H
7
NO
Acetic acid
Ethanol
Ethylacetate
Heptane
Hexane
Isopropanol
C
2
H
4
O
2
C
2
H
6
O
C
4
H
8
O
2
C
7
H
16
C
6
H
14
C
3
H
8
O
Isopentanol C
5
H
12
O
Methylethylketone C
4
H
8
O
Methanol CH
4
O
Dichlormethane
Pentane n -propanol
CH
2
CI
2
C
5
H
12
C
3
H
8
O
Pentachloroethane C
2
HCl
5
1,1,2,2-tetrachloroethane
C
2
H
2
Cl
4
Tetrachloromethane CCl
4
1,1,1-trichloroethane C
2
H
3
Cl
3
97.0
102.0
88.1
73.1
88.1
72.1
32.0
84.9
72.1
60.1
202.3
167.9
60.0
46.0
88.1
100.2
86.2
60.1
112.6
119.4
84.0
74.0
99.0
97.0
Molar mass in g/ mol
Evaporation energy in J/g
Boiling point in °C at 1013 mbar
58.1
88.1
553
595
56
37
78.1
74.1
74.1
548
620
590
80
118
82
377
264
389
389
335
322
132
62
81
35
84
60
153.8
133.4
314
318
406
–
595
473
1227
373
381
787
201
247
695
879
394
373
368
699
226
251
48
68
101
153
77
74
40
36
97
129
80
65
162
146
98
69
82
118
79
77
0.790
0.814
0.877
0.810
0.789
1.106
1.483
0.779
0.714
1.235
1.284
Density in g/cm 3
36
474
235
850
210
479
Vacuum in mbar for
40 °C boiling point
556
11
236
25
130
1.257
0.724
1.034
0.949
0.809
0.805
0.791
1.327
0.626
0.804
1.680
1.595
1.049
0.789
0.900
0.684
0.660
0.786
1.594
1.339
751
375
107
11
271
300
14
243
337
850
850
67
13
20
44
175
240
120
360
137
Operation Manual Rotavapor® R-300 77/102
10 | Appendix
Solvent
Tetrachloroethene C
2
Cl
4
THF (tetrahydrofuran)
C
4
H
8
O
Toluene
Trichloroethene
Water
Xylene (mixture) o m p
-xylene
-xylene
-xylene
C
7
H
8
C
2
HCl
3
H
2
O
C
8
H
10
C
8
H
10
C
8
H
10
C
8
H
10
Formula
BÜCHI Labortechnik AG
Molar mass in g/ mol
Evaporation energy in J/g
Boiling point in °C at 1013 mbar
165.8
72.1
234
–
121
67
Density in g/cm 3
1.623
0.889
Vacuum in mbar for
40 °C boiling point
53
374
92.2
131.3
18.0
106.2
106.2
106.2
106.2
427
264
2261
–
–
389
–
111
87
100
–
144
139
138
0.867
1.464
1.000
–
0.880
0.864
0.861
–
–
25
–
77
183
72
78/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Appendix | 10
10.2
Spare parts and accessories
u Use only genuine BUCHI consumables and spare parts in order to ensure correct, safe and reliable operation of the system.
NOTE
Any modifications of spare parts or assemblies are only allowed with the prior written permission of BUCHI.
10.2.1
Glass assembly A
Fig. 49: Glass assembly A
Operation Manual Rotavapor® R-300 79/102
10 | Appendix
10.2.2
Glass assembly V
BÜCHI Labortechnik AG
Fig. 50: Glass assembly V
80/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
10.2.3
Glass assembly C
Appendix | 10
Fig. 51: Glass assembly C
Operation Manual Rotavapor® R-300 81/102
10 | Appendix
10.2.4
Glass assembly S
BÜCHI Labortechnik AG
Fig. 52: Glass assembly S
82/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
10.2.5
Glass assembly CR
Appendix | 10
Fig. 53: Glass assembly CR
Operation Manual Rotavapor® R-300 83/102
10 | Appendix
10.2.6
Glass assembly E
001003
P+G 033508
010183
P+G 033511
005222
001002
P+G 033507
001004
040627
000646
040625
023875
023900
028096
040661
P+G 040663
003275
Fig. 54: Glass assembly E
040624
BÜCHI Labortechnik AG
048181
11062387
048321
11062186
(NS 29/32)
84/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
10.2.7
Glass assembly BY
Appendix | 10
Fig. 55: Glass assembly BY
Operation Manual Rotavapor® R-300 85/102
10 | Appendix BÜCHI Labortechnik AG
10.2.8
Accessories
Heating baths
Heating Bath B-301, 110V, not incl. Base B-300
For up to 1 liter evaporating flasks. For temperatures up to 95°C.
Meant to be used with water as heating media.
Heating Bath B-301, 230V, not incl. Base B-300
For up to 1 liter evaporating flasks. For temperatures up to 95°C.
Meant to be used with water as heating media.
Heating Bath B-301, 110V, incl. Base B-300
For up to 1 liter evaporating flasks. For temperatures up to 95°C.
Meant to be used with water as heating media.
Heating Bath B-301, 230V, incl. Basis B-300
For up to 1 liter evaporating flasks. For temperatures up to 95°C.
Meant to be used with water as heating media.
Heating Bath B-305, 110V, not incl. Base B-300
For up to 5 liter evaporating flasks. For temperatures up to 220°C.
Meant to be used with water or oil as heating media.
Heating Bath B-305, 230V, not incl. Base B-300
For up to 5 liter evaporating flasks. For temperatures up to 220°C.
Meant to be used with water or oil as heating media.
Heating Bath B-305, 110V, incl. Base B-300
For up to 5 liter evaporating flasks. For temperatures up to 220°C.
Meant to be used with water or oil as heating media.
Heating Bath B-305, 230V, incl. Base B-300
For up to 5 liter evaporating flasks. For temperatures up to 220°C.
Meant to be used with water or oil as heating media.
Adapter B-300. For Heating Bath B-305
Required when Heating Bath B-305 is used with a Rotavapor R-210,
R-215 or R II. Not compatible with Heating Bath B-301.
11B301002
11B301001
11B301102
11B301101
11B305002
11B305001
11B305102
11B305101
11061317
Accessories for heating baths
Heating bath balls. 450pcs, PP, Ø10mm
To reduce energy consumption of heating bath and for less evaporation of the heating medium. For temperatures up to 100°C.
036405
11059500 Lid. For Heating Bath B-305
To save energy and to minimize loss of water when heating bath is not in use.
Protection shield. Operator protection for heating bath
For Heating Bath B-301 and B-305.
11061402
Tubing
FEP, Ø6/8mm, transparent, per m
Use: Vacuum, cooling media.
Natural rubber, Ø6/16mm, red, per m
Use: vacuum.
Nylflex, PVC-P, Ø8/14mm, transparent, per m
Use: vacuum, cooling media, feeding (industrial Rotavapor).
027900
017622
004113
86/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Appendix | 10
PTFE, Ø4.7/5.5mm, transparent, 330 mm
Use: To introduce solvent into evaporating flask during distillation.
PTFE, Ø4.7/5.5mm, transparent, 460mm
Use: To introduce solvent into evaporating flask during distillation.
PTFE, Ø8/10mm, white, per m
Use: vacuum, feeding (industrial Rotavapor).
Silicone, Ø6/9mm, transparent, per m
Use: Cooling media.
Synthetic rubber, Ø6/13mm, black, per m
Use: vacuum.
000646
000643
027277
004133
11063244
Further accessories
AutoDest sensor. Incl. cap nut, seal GL14
For automatic distillation. Measures temperature of cooling media.
Vacuum is adjusted according to cooling capacity of condenser. Meant to be used with the Interface I-300/I-300 Pro and glass assembly
V or S.
Communication cable. Mini-DIN to RJ45, 1.5m
Connection between Vacuum Controller V-850/V-855 and Vacuum
Pump V-300 or between Vacuum Controller V-850/V-855 and
Recirculating Chiller F-3xx.
Condensate trap. Grey, TPE, for condenser V, hose connector
Ø8mm
Collects and drains condensate which may accumulate at the condenser.
Condensate trap. Green, TPE, for condenser V, hose connector
Ø8mm
Collects and drains condensate which may accumulate at the condenser.
Cooling water valve. 24VAC
Valve opens cooling water feed during distillation. Meant to be used with a vacuum Controller/interface.
Extraction thimbles, set. 25pcs, 200mL, cellulose
For Soxhlet extraction unit.
Flask holder. EPDM, slip free
Holder for round-bottom flasks (50-5000mL).
Flask holders, set. 5pcs, EPDM, slip free
Holder for round-bottom flasks (50-5000mL).
Foam sensor. Incl. holder
Prevents sample from foaming into the condenser by aeration of system temporarily. Meant to be used with the
Interface I-300/I-300 Pro.
Holder. For extraction unit, steel, 750mm, Ø12mm
Lab grease. Glisseal 40 (60g)
To grease joints in order to increase tightness of system.
LegacyBox. incl. accessory set
Interface between Interface I-300/I-300 Pro (with VacuBox) to peripherals of older generations (Vacuum Pump V-7xx, Recirculating
Chiller F-1xx).
11059225
11060649
11062955
11061985
031356
018106
048618
11059916
11061167
011904
048197
11061166
Operation Manual Rotavapor® R-300 87/102
10 | Appendix BÜCHI Labortechnik AG
Level sensor. Incl. O-ring, cable, rubber band
Prevents an overflow in the receiving flask of condenser/secondary cold trap. Placed on receiving flask. Meant to be used with the Interface
I-300/I-300 Pro.
11060954
Set earthquake fastener. Lug for backside
To fasten device on lab bench.
Vacuum connection. Incl. drain valve, hose barb ∅ 8mm, KS35/20
Connection piece for aeration of the system, placed between condenser and receiving flask.
11062386
001006
11060706 Vacuum valve. Magnetic valve, 24V/4W, Mini-DIN, 1.5m
Flow valve without flask, meant to be used with a centralized vacuum source or an unregulated vacuum pump. Meant to be used with the
Interface I-300/I-300 Pro.
Vapor temperature sensor. Incl. cap nut, seal GL14
Measures the vapor temperature inside the system. Meant to be used with the Interface I-300/I-300 Pro.
Water jet pump. Plastic
Used when tap water is used to generate vacuum.
11060707
002913
Water jet pump, B-764. Magnetic valve, FFKM, 24V
Used when tap water is used to generate vacuum. Not inclusive:
Cooling water valve. Meant to be used with a vacuum
Controller/interface.
Water jet pump, B-767. Magnetic valve (2pcs), FFKM, 24V
Used when tap water is used to generate vacuum. Inclusive: Cooling water valve. Meant to be used with a vacuum Controller/interface.
Water regulation nozzle. Flow regulator, incl. hose clamp, sieve
Used when tap water is used to generate vacuum. Reduces water consumption.
031358
031357
011606
88/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Appendix | 10
Glassware
Glass assemblies
Glass assembly V. Vertical condenser, 1500cm2
For standard distillations, used with recirculating chiller or tap water.
Features: Cleaning hole on top. Content: 1 L receiving flask, required tubings, ball joint clamp, stopcock, feeding tubing. Not inclusive:
Evaporating flask, vapor duct, vacuum gasket, holder.
Glass assembly A. Diagonal condenser, 1500cm2, P+G
For standard distillations, used with recirculating chiller or tap water.
Features: Cleaning hole on top. Content: 1 L receiving flask (P+G), required tubings, ball joint clamp, stopcock, feeding tubing. Not inclusive: Evaporating flask, vapor duct, vacuum gasket, holder.
Glass assembly BY. Vertical intensive condenser, reflux,
1300cm2, P+G
For particularly efficient condensation with double jacket condenser as well as for reflux distillations with distributor and shut-off valve. Used with recirculating chiller or tap water. Features: Double jacket condenser. Additional joint on top of the condenser for flexible expansion
(SJ29/32). Connection for vapor temperature sensor. Content: 1 L receiving flask, required tubings, ball joint clamp, stopcock, feeding tubing, distributor. Not inclusive: Evaporating flask, vapor duct, vacuum gasket, holder.
Glass assembly BY. Vertical intensive condenser, reflux,
1300cm2, P+G
For particularly efficient condensation with double jacket condenser as well as for reflux distillations with distributor and shut-off valve. Used with recirculating chiller or tap water. Features: Double jacket condenser. Additional joint on top of the condenser for flexible expansion
(SJ29/32). Connection for vapor temperature sensor. Content: 1 L receiving flask (P+G), required tubings, ball joint clamp, stopcock, feeding tubing, distributor. Not inclusive: Evaporating flask, vapor duct, vacuum gasket, holder.
Glass assembly C. Cold trap, 500cm2
For distillations of low-boiling point solvents. No need of cooling liquid, but e.g. dry ice. Content: 1 L receiving flask, ball joint clamp, stopcock, feeding tubing. Not inclusive: Evaporating flask, vapor duct, vacuum gasket, holder.
Glass assembly C. Cold trap, 500cm2, P+G-LT
For distillations of low-boiling point solvents. No need of cooling liquid, but e.g. dry ice. Application temperature: -70 to 40°C. Content: 1 L receiving flask (P+G-LT), ball joint clamp, stopcock, feeding tubing. Not inclusive: Evaporating flask, vapor duct, vacuum gasket, holder.
Glass assembly CR. Cold trap reflux, 500cm2
For reflux distillations with distributor and shut-off valve as well as for distillation of low-boiling point solvents. No need of cooling liquid, but e.g. dry ice. Content: 1 L receiving flask, ball joint clamp, stopcock, feeding tubing, distributor. Not inclusive: Evaporating flask, vapor duct, vacuum gasket, holder.
048168
048169
048176
048297
040640
040642
048292
Operation Manual Rotavapor® R-300 89/102
10 | Appendix
90/102
BÜCHI Labortechnik AG
Glass assembly CR. Cold trap reflux condenser, 500cm2, P+G-LT
For reflux distillations with distributor and shut-off valve as well as for distillation of low-boiling point solvents. No need of cooling liquid, but e.g. dry ice. Application temperature: -70 to 40°C. Content: 1 L receiving flask, ball joint clamp, stopcock, feeding tubing, distributor.
Not inclusive: Evaporating flask, vapor duct, vacuum gasket, holder.
Glass assembly E. Expansion condenser, 1500cm2
Optimised for distillations of foaming substances and bumping sample solutions. Used with recirculating chiller or tap water. Features:
Descending condenser with expansion vessel. Cleaning hole on top.
Connection for vapor temperature sensor. Content: 1 L receiving flask, required tubings, ball joint clamp, stopcock, feeding tubing, holder. Not inclusive: Evaporating flask, vapor duct, vacuum gasket.
Glass assembly E. Expansion condenser, 1500cm2, P+G
Optimised for distillations of foaming substances and bumping sample solutions. Used with recirculating chiller or tap water. Features:
Descending condenser with expansion vessel. Cleaning hole on top.
Connection for vapor temperature sensor. Content: 1 L receiving flask
(P+G), required tubings, ball joint clamp, stopcock, feeding tubing, holder. Not inclusive: Evaporating flask, vapor duct, vacuum gasket.
Glass assembly S. Vertical condenser reflux, 1500cm2
For reflux distillations with distributor and shut-off valve. Used with recirculating chiller or tap water. Features: Cleaning hole on top.
Connection for vapor temperature sensor. Inner glass tube. Content:
1 L receiving flask, required tubings, ball joint clamp, stopcock, feeding tubing, distributor. Not inclusive: Evaporating flask, vapor duct, vacuum gasket, holder.
048293
11061112
11061113
048290
Glass assembly S. Vertical condenser reflux, 1500cm2, P+G
For reflux distillations with distributor and shut-off valve. Used with recirculating chiller or tap water. Features: Cleaning hole on top.
Connection for vapor temperature sensor. Inner glass tube. Content:
1 L receiving flask (P+G), required tubings, ball joint clamp, stopcock, feeding tubing, distributor. Not inclusive: Evaporating flask, vapor duct, vacuum gasket, holder.
Glass assembly V. Vertical condenser, 1500cm2
For standard distillations, used with recirculating chiller or tap water.
Features: Large cleaning hole on top (SVL22). Connection for vapor temperature sensor. Inner glass tube. Inner glass plate. Content: 1 L receiving flask, required tubings, ball joint clamp, stopcock, feeding tubing. Not inclusive: Evaporating flask, vapor duct, vacuum gasket, holder.
048291
11062432
Glass assembly A. Vertical condenser, 1500cm2, P+G
For standard distillations, used with recirculating chiller or tap water.
Features: Large cleaning hole on top (SVL22). Connection for vapor temperature sensor. Inner glass tube. Inner glass plate. Content: 1 L receiving flask (P+G), required tubings, ball joint clamp, stopcock, feeding tubing. Not inclusive: Evaporating flask, vapor duct, vacuum gasket, holder.
11062433
Accessories for glass assemblies
Condenser holder. For Glass assembly V/C/S/CR/BY
Content: Holding rod, rubber band, cross sleve.
048180
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
Extraction unit Soxhlet. 200mL, incl. extraction part, reduction part
For Soxhlet extraction applications. Meant to be used with glass assembly S.
Extraction unit Soxhlet. 500mL, incl. extraction part, reduction part
For Soxhlet extraction applications. Meant to be used with glass assembly S.
Bump trap adapters
Glass, NS24/40, 175mm
Glass, NS29/32, 160mm
Glass, Reitmeyer, NS24/40, 150mm
Glass, Reitmeyer, NS29/32, 135mm
Evaporating flasks
Glass, NS24/29, 1000mL
Glass, NS24/29, 100mL
Glass, NS24/29, 2000mL
Glass, NS24/29, 250mL
Glass, NS24/29, 50mL
Glass, NS24/40, 1000mL
Glass, NS24/40, 1000mL, P+G
Glass, NS24/40, 100mL
Glass, NS24/40, 2000mL
Glass, NS24/40, 2000mL, P+G
Glass, NS24/40, 250mL
Glass, NS24/40, 3000mL
Glass, NS24/40, 3000mL, P+G
Glass, NS24/40, 4000mL, P+G
Glass, NS24/40, 5000mL, P+G
Glass, NS24/40, 500mL
Glass, NS24/40, 500mL, P+G
Glass, NS24/40, 50mL
Glass, NS29/32, 1000mL
Glass, NS29/32, 1000mL, P+G
Glass, NS29/32, 100mL
Glass, NS29/32, 100mL, P+G
Glass, NS29/32, 2000mL
Glass, NS29/32, 2000mL, P+G
Glass, NS29/32, 250mL
Glass, NS29/32, 250mL, P+G
Glass, NS29/32, 3000mL
Operation Manual Rotavapor® R-300
Appendix | 10
011744
011745
11056919
11056920
036577
036576
046596
008758
025261
008750
000435
020729
000432
033404
000436
025323
000433
025520
000437
008761
000473
008764
008753
000472
000440
020730
008751
008765
025262
008754
008767
025263
047992
91/102
10 | Appendix
92/102
Glass, NS29/32, 3000mL, P+G
Glass, NS29/32, 4000mL
Glass, NS29/32, 4000mL, P+G
Glass, NS29/32, 5000mL, P+G
Glass, NS29/32, 500mL
Glass, NS29/32, 500mL, P+G
Glass, NS29/32, 50mL
Glass, NS29/32, 50mL, P+G
Glass, NS29/42, 1000mL
Glass, NS29/42, 1000mL, P+G
Glass, NS29/42, 100mL
Glass, NS29/42, 2000mL
Glass, NS29/42, 250mL
Glass, NS29/42, 3000mL
Glass, NS29/42, 3000mL, P+G
Glass, NS29/42, 500mL
Glass, NS29/42, 50mL
Glass, NS34/35, 1000mL
Glass, NS34/35, 500mL
Drying flasks
Glass, NS24/40, 1000mL
With 4 indents for better mixing/drying.
Glass, NS24/40, 2000mL
With 4 indents for better mixing/drying.
Glass, NS24/40, 500mL
With 4 indents for better mixing/drying.
Glass, NS29/32, 1000mL
With 4 indents for better mixing/drying.
Glass, NS29/32, 2000mL
With 4 indents for better mixing/drying.
Glass, NS29/32, 500mL
With 4 indents for better mixing/drying.
Beaker flasks
Glass, NS29/32, 1500mL, for evaporation
Glass, NS24/40, 1500mL, for evaporation
Glass, NS29/32, 1500mL, for drying
With 4 indents for better mixing/drying.
Glass, NS24/40, 1500mL, for drying
With 4 indents for better mixing/drying.
Glass, NS29/32, 500mL, for evaporation
Glass, NS24/40, 500mL, for evaporation
11063156
11063157
11063160
11063161
11063154
11063155
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
025324
047991
047993
046583
000434
025322
000431
033405
008762
025517
008737
008769
008738
008770
027346
008739
008736
008763
008759
000420
011580
011579
000453
000454
000452
BÜCHI Labortechnik AG
Glass, NS29/32, 500mL, for drying
With 4 indents for better mixing/drying.
Glass, NS24/40, 500mL, for drying
With 4 indents for better mixing/drying.
Receiving flasks
Glass, KS35/20, 1000mL
Glass, KS35/20, 1000mL, P+G
Glass, KS35/20, 1000mL, P+G-LT
Application temperature: -70 to 40°C.
Glass, KS35/20, 100mL
Glass, KS35/20, 2000mL
Glass, KS35/20, 2000mL, P+G
Glass, KS35/20, 2000mL, P+G-LT
Application temperature: -70 to 40°C.
Glass, KS35/20, 250mL
Glass, KS35/20, 250mL, P+G
Glass, KS35/20, 250mL, P+G-LT
Application temperature: -70 to 40°C.
Glass, KS35/20, 3000mL
Glass, KS35/20, 3000mL, P+G
Glass, KS35/20, 3000mL, P+G-LT
Application temperature: -70 to 40°C.
Glass, KS35/20, 500mL
Glass, KS35/20, 500mL, P+G
Glass, KS35/20, 500mL, P+G-LT
Application temperature: -70 to 40°C.
Glass, KS35/20, 50mL
Receiving flask with drain valve. Glass, BJ35/20, 1000mL, P+G,
PTFE
Vapor ducts
Ø26mm, NS24/40, incl. Combi-Clip
For Glass assembly A.
Ø26mm, NS24/40, incl. Combi-Clip
Analytical, long. For glass assembly V, C, S, E, BY and CR.
Ø26mm, NS29/32, incl. Combi-Clip
For Glass assembly A.
Ø26mm, NS29/32, incl. Combi-Clip
Analytical, long. For glass assembly V, C, S, E, BY and CR.
Ø26mm, NS29/42, incl. Combi-Clip
For Glass assembly A.
Ø26mm, NS29/42, incl. Combi-Clip
For Glass assembly V, C, S, E, BY and CR.
Appendix | 10
11063158
11063159
000425
020728
040775
000422
000426
025265
040776
000423
11060907
11060908
000427
025266
040777
000424
025264
040774
000421
036919
11062268
11062466
11062267
11062465
11062269
11062464
Operation Manual Rotavapor® R-300 93/102
10 | Appendix BÜCHI Labortechnik AG
Ø26mm, NS29/42, incl. Combi-Clip
Analytical, long. For glass assembly V, C, S, E, BY and CR.
Ø22mm, NS29/32, incl. Combi-Clip
Meant to be used with KD22. For glass assembly V, C, S, E, BY and
CR.
Ø26mm, NS24/29, incl. Combi-Clip
For Glass assembly V, C, S, E, BY and CR.
Ø26mm, NS24/40, incl. Combi-Clip
For Glass assembly V, C, S, E, BY and CR.
Ø26mm, NS29/32, incl. Combi-Clip
For Glass assembly V, C, S, E, BY and CR.
Vapor duct with frit. Ø26mm, NS29/32, incl. Combi-Clip
For powder drying. To prevent powder from getting into the condenser.
For glass assembly V, C, S, E, BY and CR.
11062467
11062910
11062909
11062187
11062186
11057297
Stopcocks
For condenser C/CR, glass, NS18.8/38
For aeration of the system. For cold trap outer part.
Professional, glass, NS18.8/38
For aeration of the system. Less cross-contamination compared to standard-stopcock (040627).
PTFE, incl. 3-way valve
For feeding of solvents and aeration of the system. For applications when grease should be avoided. Used instead of standard-stopcock
(040627). Content: Inlet tubing 300mm, backfeed tubing 600mm, cap nut GL10.
PTFE, NS18.8/38
For aeration of the system. For applications when grease should be avoided. Used instead of standard-stopcock (040627).
Standard, glass, NS18.8/38
For aeration of the system.
040628
000637
11058814
023896
040627
Distillation spiders
Glass, NS24/40, incl. 100mL flask (5pcs)
Glass, NS24/40, incl. 20mL cyl. flask (20pcs)
Glass, NS24/40, incl. 50mL flask (5pcs)
Glass, NS29/32, incl. 100mL flask (5pcs)
Glass, NS29/32, incl. 20mL cyl. flask (12pcs)
Glass, NS29/32, incl. 20mL cyl. flask (20pcs)
Glass, NS29/32, incl. 20mL cyl. flask (6pcs)
Glass, NS29/32, incl. 50mL flask (5pcs)
011575
011578
011574
001333
001335
001336
001334
001332
10.2.9
Wear parts
Vacuum gasket
Vacuum gasket. WD26, PTFE, FDA-compliant 048021
94/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG
Seals
For cap nut GL14 to FEP, EPDM
Set. 10pcs, for hose barbs GL14, EPDM, black
Set. 10pcs, for hose barbs GL14, FPM, green
Set. 20pcs, for hose barbs GL14, silicone, red
Hose barbs
Bent, GL14, incl. silicone seal
Set. . 2pcs, bent (1), straight (1), GL14, silicone seal
Content: Hose barbs, cap nuts, seals.
Set. 3pcs, bent, GL14, silicone seal
Content: Hose barbs, seals.
Set. 4pcs, bent GL14, silicone seal
Content: Hose barbs, cap nuts, seals.
Set. 4pcs, bent, GL14, EPDM seal
Content: Hose barbs, cap nuts, seals.
Set. 4pcs, bent, GL14, FPM seal
Content: Hose barbs, cap nuts, seals.
Set. 4pcs, straight, GL14, EPDM seal
Content: Hose barbs, cap nuts, seals.
Set. 4pcs, straight, GL14, FPM seal
Content: Hose barbs, cap nuts, seals.
Set. 4pcs, straight, GL14, silicone seal
Content: Hose barbs, seals.
Set. 6pcs, bent (4), straight (2), GL14, silicone seal
Content: Hose barbs, cap nuts, seals.
Further wear parts
Cap nut. Screw cap with hole GL10
Cap nuts, set. 10pcs, screw cap with hole GL14, seal EPDM
Content: Hose barbs, cap nuts, seals.
Cap nuts, set. 10pcs screw cap with hole GL14
O-ring. FKM, 40.9/2.6mm, for reflux insert
O-ring. FPM, for cap nut GL10, Ø3.00/2.70mm
Screw caps, set. 5pcs, GL14
Set screwings. Hose barbs and seals GL14, set
Content: Hose barbs bent 4pcs, hose barbs straight 1pc, cap nuts
4pcs, screw caps 2pcs, seals EPDM 3pcs.
10.2.10
Spare parts
Glassware
Beaker flask. Glass, 1500mL, for evaporation
Beaker flask. Glass, 1500mL, for drying
With 4 indents for better mixing/drying.
Appendix | 10
038225
040029
040040
040023
023875
041999
041956
048078
023900
040624
11061921
11059186
11059269
018916
041939
041987
037287
043129
040295
043128
040296
037642
038000
Operation Manual Rotavapor® R-300 95/102
10 | Appendix
96/102
BÜCHI Labortechnik AG
Beaker flask. Glass, 500mL, for evaporation
Beaker flask. Glass, 500mL, for drying
With 4 indents for better mixing/drying.
Coupling piece. Glass, NS29/32
For beaker flask 1500mL.
Coupling piece. Glass, NS24/40
For beaker flask 1500mL.
11059185
11059268
11059187
11059363
Coupling piece. Glass, NS29/32
For beaker flask 500mL.
Coupling piece. Glass, NS24/40
For beaker flask 500mL.
Distillation spider. Glass, NS29/32 (for 20 flasks), not incl. flasks
11059043
11059362
Distillation spider. Glass, NS24/40 (for 5 flasks), not incl. flasks
Distillation spider. Glass, NS29/32 (for 12 flasks), not incl. flasks
Distillation spider. Glass, NS29/32 (for 5 flasks), not incl. flasks
000476
000466
000475
000471
Distillation spider. Glass, NS29/32 (for 6 flasks), not incl. flasks 000474
Distribution head. For assembly S/CR/BY, P+G, incl. cap nut GL10 040658
Distribution head. For glass assembly E, incl. cap nut GL10 040661
Distribution head. For glass assembly E, P+G, incl. cap nut GL10 040663
Distribution head. For glass assembly S/CR/BY, incl. cap nut GL10 040657
Evaporating flask. Glass, NS24/40, 5000mL, P+G 046586
Evaporating flask. Glass, NS29/32, 5000mL
Expansion vessel. For assembly E, glass, P+G, incl. screw cap
GL14
Expansion vessel. For Glass assembly E, glass, incl. screw cap
GL14
U-tube. For assembly E, Glass, incl. screw cap GL14
U-tube. For assembly E, glass, P+G, incl. screw cap GL14
046573
033507
001002
001003
033508
Seals
For beaker flask 1500mL, Ø100mm, incl. O-ring
PTFE coated seal for beaker flask.
For beaker flask 500mL, Ø68mm, incl. O-ring
PTFE coated seal for beaker flask.
Set. For condenser C/CR, O-ring EPDM/PTFE
Seal between cold trap outer part and cold finger.
Set. For Woulff bottle/valve unit
Content: O-ring (048406, 5pcs), O-ring (047169, 5pcs).
Set. For Woulff bottle/valve unit
Content: O-ring (048406, 5pcs), O-ring (047169, 5pcs), spare parts for valve unit (047258), seal (047165).
034152
034772
027462
045544
045545
Condensers
Condenser A. Diagonal condenser, 1500cm2 046988
Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Appendix | 10
Condenser A. Diagonal condenser, 1500cm2, P+G
Condenser BY. Double jacket, 1300cm2, P+G
Condenser BY. Double jacket, 1300cm2
Condenser C. Cold trap, 500cm2
Condenser C. Cold trap, 500cm2.P+G-LT
Application temperature: -70 to 40°C.
Condenser CR. Cold trap reflux, outer part
Condenser CR. Cold trap reflux, outer part, P+G-LT
Application temperature: -70 to 40°C.
Condenser CR. Cold trap reflux, 500cm2
Condenser CR. Cold trap reflux, 500cm2, P+G-LT
Application temperature: -70 to 40°C.
Condenser E. Expansion, 1500cm2
Condenser E. Expansion, 1500cm2, P+G
Condenser S. Vertical condenser reflux, 1500cm2
Condenser S. Vertical condenser reflux, 1500cm2, P+G
Condenser V. Vertical condenser, 1500cm2
Condenser V. Vertical condenser, 1500cm2, P+G
047976
035040
048177
040645
040646
011228
025614
011511
033478
010183
033511
040651
040653
11059368
11059369
Further spare parts
Ball joint clamp. For KS25/20
Not inclusive: Rubber band (032013).
Beaker clasp. Flange screwed connection
For beaker flask 1500mL
Beaker clasp. Flange screwed connection
For beaker flask 500mL
Cold finger. For condenser C/CR
Cold trap mantle. For condenser C
Cold trap mantle. For condenser C, P+G-LT
Application temperature: -70 to 40°C.
Condenser holder. For Glass assembly E
Content: Holding rod, bride, cross sleeve.
Cross sleeve. To fasten condenser clamp
Not inclusive: Rubber band (032013)
003275
11059851
11059810
000672
040641
040643
048181
027344
Deflector rings, set. Drain sleeve, EPDM, black, Ø41/55mm
Drains off condensate which may accumulate at the condenser.
Drain disc. PTFE, Ø5.1/14mm
040822
040625
Flange screwed connection. For Glass assembly V/C/A
Content: Flange nut, pressure spring.
11062387
Flange screwed connection-reflux. For Glass assembly E/S/BY/CR
Content: Flange nut, reflux part, pressure spring, O-ring FKM.
048080
Fuses, set. 10pcs, 6.3AT, 20mm, Ø5mm 022561
Fuses, set. 10pcs, 12.5AT, 20mm, Ø5mm 047939
Heating Bath B-300 Base. For Heating Bath B-301 and B-305, 110V 11B30002
Operation Manual Rotavapor® R-300 97/102
10 | Appendix BÜCHI Labortechnik AG
Heating Bath B-300 Base. For Heating Bath B-301 and B-305, 230V 11B30001
Holder. Clamp for glass assembly E
Lid. For condenser C/CR, PETP
048125
027479
Manometer with needle valve. Incl. vacuum gauge, not incl. holder 047391
Navigation knob. Ø30mm, green/grey, incl. knob case, cover
For Rotavapor R-300, Heating Bath B-300 Base, Interface I-300/I-300
Pro and Recirculating Chiller F-305/F-308/F-314.
11059157
Receiving vessel. For Woulff bottle, GL40, 125mL, P+G
Rubber band. To fasten condenser on holder
Sieve. For water control valve (011606), Ø18mm
Shut-off valve. For distribution head of glass assembly S/CR/BY
For reflux reactions, for interruption of condensation.
T-piece. Incl. cap nut (3pcs) GL14
Tubing. PTFE, Ø3/4mm, white, 600mm
Use: Feeding.
Vacuum connection. For glass assembly BY, vacuum piece
To close the top hole (NS29/32) of the condenser if no expansion is used. Openings with screw cap SVL15 (on top) and with cap nut GL14
(sideward).
Vacuum connector. For glass assembly E, incl. hose barb GL14
047233
032013
011514
040626
038190
028096
035026
001004
10.3
List of abbreviations
Abbreviation Meaning
ADR Accord européen relatif au transport international des marchandises dangereuses par route (European Agreement concerning the
International Carriage of Dangerous Goods by Road)
DKD Deutscher Kalibrierdienst (German Calibration Service)
EPDM
FEP
FFKM
FPM
GGVE
Ethylene propylene diene monomer
Fluorinated ethylene propylene
Perfluoro-elastomer
Fluorinated propylene monomer
Gefahrgutverordnung Eisenbahn (German Hazardous Goods Regulations for Railways)
GGVS
NBR
PBT
PETP
PTFE
RID
Gefahrgutverordnung Strasse (German Hazardous Goods Regulations for Road Transport)
Nitrile butadiene rubber
Polybutylene terephthalate
Polyethylene terephthalate
Polytetrafluoroethylene
Règlement concernant le transport international ferroviaire de marchandises dangereuses (Regulations concerning the International Carriage of Dangerous Goods by Rail)
98/102 Operation Manual Rotavapor® R-300
BÜCHI Labortechnik AG Appendix | 10
10.4
Health and safety approval
To guarantee the health and safety of our staff and to comply with the law and the regulations for handling hazardous materials, for the purposes of health and safety at work and safe disposal of waste, no products may be sent back to BÜCHI
Labortechnik AG or repaired unless we have received the declaration below, completed and signed.
Products sent to us will not be accepted for repair until we have received this declaration.
u u u u u
Copy the form overleaf and complete it.
Make sure that you know the full details of the substances with which the device has been in contact and that all questions have been answered fully and correctly.
Send the completed form to us in advance by post or fax. The declaration must reach us before the device.
Enclose a copy of the declaration with the device.
If the product is contaminated, inform the carrier (in accordance with
GGVE/GGVS/RID/ADR).
If the declaration is missing or the procedure described is not followed, the repairs will be delayed. We ask for your understanding and cooperation with regard to these measures.
Operation Manual Rotavapor® R-300 99/102
10 | Appendix BÜCHI Labortechnik AG
10.5
Health and safety
Declaration regarding the safety, hazards and safe disposal of waste
To guarantee the health and safety of our staff and to comply with the law and the regulations for handling hazardous materials, regarding health and safety at work, and to comply with safety regulations, health and safety requirements and requirements for safe disposal of waste such as chemical waste, chemical residues or solvents, the form below must be fully completed and signed whenever devices or faulty components are to be sent back to our factory.
Products or components will not be accepted if this declaration has not been provided.
Device
Model: Part/Device no.:
Declaration for non-hazardous materials
We hereby assure that the products returned have not been used in the laboratory and are new.
have not been in contact with toxic, corrosive, biologically active, explosive, radioactive or other hazardous materials.
are not contaminated. The solvents or residues of the substances pumped have been removed.
Declaration for hazardous materials
In respect of the products returned, we hereby assure that all substances (toxic, corrosive, biologically active, explosive, radioactive or otherwise hazardous) that have been pumped by the products or have otherwise been in contact with the products are listed below.
the products have been cleaned, decontaminated, sterilised inside and outside and all inlets and outlets are sealed.
List of hazardous materials that have been in contact with the products:
Chemical, material Hazard category
Final declaration We hereby declare that
we are fully conversant with the substances that have been in contact with the products and have answered all questions correctly.
we have taken all measures necessary to prevent potential hazards in respect of the products returned.
Company name or stamp:
Place, date:
Name (block letters), position
(block letters):
Signature:
100/102 Operation Manual Rotavapor® R-300
Quality in your hands
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Key features
- Vacuum distillation for efficient evaporation
- Rotating flask for increased surface area and mixing
- Precise temperature control with heating bath
- Cooling condenser for efficient solvent recovery
- Multiple heating bath sizes for different flask capacities
- Overheat safety cut-offs