Rotavapor® R100 Operation Manual

Rotavapor® R100 Operation Manual
11593663 en
Rotavapor® R­100
Operation Manual
Imprint
Product Identification:
Operation Manual (Original) Rotavapor® R­100
11593663 en
Publication date:
12.2014, Version B
BÜCHI Labortechnik AG
Meierseggstrasse 40
Postfach
CH­9230 Flawil 1
E­Mail: [email protected]
BUCHI reserves the right to make changes to the manual as deemed necessary in the light of experi­
ence; especially in respect to structure, illustrations and technical detail.
This manual is copyrighted. Information from it may not be reproduced, distributed, or used for competi­
tive 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
Contents
1
About this document........................................................................................................... 5
1.1
1.2
1.3
1.4
Warning notices in this document........................................................................................................ 5
Symbols ............................................................................................................................................... 5
1.2.1 Warning symbols ..................................................................................................................... 5
1.2.2 Mandatory directive symbols ................................................................................................... 6
1.2.3 Other symbols.......................................................................................................................... 6
Available languages............................................................................................................................. 6
Trademarks.......................................................................................................................................... 6
2
Safety.................................................................................................................................... 7
2.1
2.2
2.3
2.4
2.5
2.6
Intended use ........................................................................................................................................ 7
Use other than that intended ............................................................................................................... 7
Staff qualification ................................................................................................................................. 8
Residual risks ...................................................................................................................................... 8
2.4.1 Dangerous vapors.................................................................................................................... 8
2.4.2 High internal pressure.............................................................................................................. 9
2.4.3 Hot surfaces and liquids........................................................................................................... 9
2.4.4 Glass breakage........................................................................................................................ 9
2.4.5 Rotating parts........................................................................................................................... 9
2.4.6 Faults during operation ............................................................................................................ 9
Personal protective equipment ............................................................................................................ 9
Modifications...................................................................................................................................... 10
3
Product description........................................................................................................... 11
3.1
3.2
Description of function ....................................................................................................................... 11
Configuration ..................................................................................................................................... 12
3.2.1 Front view .............................................................................................................................. 12
3.2.2 Rear view ............................................................................................................................... 13
3.2.3 Heating bath user interface.................................................................................................... 13
3.2.4 Typical application ................................................................................................................. 14
3.2.5 Type plate .............................................................................................................................. 15
3.2.6 Warning symbols on the device ............................................................................................. 16
Specifications supplied ...................................................................................................................... 16
Technical data ................................................................................................................................... 17
3.4.1 Rotavapor® R­100 ................................................................................................................. 17
3.4.2 Heating bath B­100 ................................................................................................................ 17
3.4.3 Ambient conditions................................................................................................................. 18
3.4.4 Materials ................................................................................................................................ 18
Safety features................................................................................................................................... 19
3.5.1 Overheat cut­out .................................................................................................................... 19
3.5.2 Protection against electrical overload .................................................................................... 19
3.5.3 Clips and holders ................................................................................................................... 19
3.5.4 Glassware .............................................................................................................................. 19
3.5.5 Optional accessories.............................................................................................................. 19
3.3
3.4
3.5
4
Transport and storage ...................................................................................................... 20
4.1
4.2
Transport ........................................................................................................................................... 20
Storage .............................................................................................................................................. 20
Operation Manual Rotavapor® R­100
iii
Contents
BÜCHI Labortechnik AG
5
Installation.......................................................................................................................... 21
5.1
5.2
5.3
5.4
5.5
5.6
5.7
5.8
5.9
Installation site ................................................................................................................................... 21
Mounting the rotary drive unit ............................................................................................................ 21
Fitting the vapor duct and condenser ................................................................................................ 22
Fitting the glass stopcock .................................................................................................................. 23
Connecting the vacuum and cooling media tubing ............................................................................ 24
Electrical connections ........................................................................................................................ 25
Overview of connections.................................................................................................................... 25
Setting up and filling the heating bath................................................................................................ 26
Quick check ....................................................................................................................................... 26
6
Operation............................................................................................................................ 27
6.1
Preparations ...................................................................................................................................... 27
6.1.1 Preparing the heating bath..................................................................................................... 27
6.1.2 Fitting the evaporating flask ................................................................................................... 28
6.1.3 Adjusting immersion angle of evaporating flask..................................................................... 29
6.1.4 Fitting the receiving flask ....................................................................................................... 30
6.1.5 Vertical adjustment ................................................................................................................ 30
Performing distillation ........................................................................................................................ 32
6.2.1 Raising and lowering the evaporating flask ........................................................................... 33
6.2.2 Adjusting distillation conditions .............................................................................................. 34
6.2.3 Optimization distillation .......................................................................................................... 35
6.2.4 Feeding solvent during distillation.......................................................................................... 36
Finishing distillation............................................................................................................................ 37
6.3.1 Removing the evaporating flask............................................................................................. 37
6.3.2 Removing the receiving flask ................................................................................................. 38
6.2
6.3
7
Cleaning and servicing ..................................................................................................... 39
7.1
7.2
7.3
7.4
7.5
7.6
Inspecting and cleaning the vapor duct ............................................................................................. 39
Checking the system for leaks........................................................................................................... 39
Checking seals .................................................................................................................................. 40
Cleaning the condenser..................................................................................................................... 40
Cleaning the heating bath.................................................................................................................. 41
Removing solvent accumulations ...................................................................................................... 41
8
Help with faults .................................................................................................................. 42
8.1
8.2
Faults, possible causes and remedies............................................................................................... 42
Remedy ............................................................................................................................................. 44
8.2.1 Resetting overheat safety cut­out .......................................................................................... 44
8.2.2 Replacing the fuse ................................................................................................................. 45
9
Taking out of service and disposal.................................................................................. 46
9.1
9.2
Taking out of service.......................................................................................................................... 46
Disposal ............................................................................................................................................. 46
10
Appendix ............................................................................................................................ 47
10.1
10.2
Solvent table ...................................................................................................................................... 47
Spare parts and accessories ............................................................................................................. 48
10.2.1 Glass apparatus V ................................................................................................................. 49
10.2.2 Glass apparatus C ................................................................................................................. 50
10.2.3 Accessories............................................................................................................................ 51
10.2.4 Wear parts ............................................................................................................................. 55
10.2.5 Spare parts ............................................................................................................................ 56
List of abbreviations........................................................................................................................... 57
Health and safety approval ................................................................................................................ 57
Health and safety............................................................................................................................... 58
10.3
10.4
10.5
iv
Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
1
About this document | 1
About this document
These operating instructions describe the Rotavapor® R­100 at the time supplied.
They are an integral part of the product and contain important information that is nec­
essary for safe operation and maintenance.
These operating instructions apply to all variants of the Rotavapor® R­100 and are in­
tended primarily for laboratory staff.
u To ensure safe and trouble­free operation, read these operating instructions before
starting up the device and follow the guidance they contain.
u Keep the operating instructions somewhere near to the device.
u 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 In­
ternet 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.
1.2
Signal word
Meaning
DANGER
Indicates a danger with a high level of risk which could result in
death or serious injury if not prevented.
WARNING
Indicates a danger with a medium level of risk which could result in
death or serious injury if not prevented.
CAUTION
Indicates a danger with a low level of risk which could result in mi­
nor or medium­severity injury if not prevented.
IMPORTANT
Indicates a danger that could result in damage to property.
Symbols
The following symbols may be displayed in this instruction manual or on the device:
1.2.1
Warning symbols
Symbol
Operation Manual Rotavapor® R­100
Meaning
Symbol
Meaning
General warning
Corrosive substance
Dangerous electrical voltage
Flammable substance
Biological hazard
Potentially explosive atmos­
phere
Breakable items
Dangerous gases
5/60
1 | About this document
BÜCHI Labortechnik AG
Symbol
1.2.2
Symbol
Meaning
Hot surface
Health­harming or irritant
substances
Risk of hand injury
Strong magnetism
Mandatory directive symbols
Symbol
1.2.3
Meaning
Meaning
Symbol
Meaning
Wear safety goggles
Wear protective clothing
Wear protective gloves
Heavy load, do not lift without
assistance
Other symbols
NOTE
This symbol draws attention to useful and important information.
R This character draws attention to a requirement that must be met before the in­
structions 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.
1.3
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.
1.4
Trademarks
Product names and registered or unregistered trademarks that are used in this instruc­
tion manual are used only for identification and remain the property of the owner in
each case.
Rotavapor® is a registered trademark of BÜCHI Labortechnik AG.
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Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
Safety | 2
2
Safety
2.1
Intended use
The Rotavapor® R­100 is intended for evaporating and condensing solvents. It can be
used in laboratories and production facilities for the following operations:
— Evaporating and condensing solvents and suspensions
— Synthesis and purification of refined chemicals
— Recycling and concentration of solvents
— Recrystallization
— Drying of powders and granulates
2.2
Use other than that intended
Use of any kind other than that described in the section Chapter 2.1 "Intended use",
page 7 and any application that does not comply with the technical specifications
(see Chapter 3.4 "Technical data", page 17) 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 explosion­safe 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
— Distillation of oil
— Drying hard, brittle substances (e.g. stone or soil samples) that could damage the
evaporating flask
— Shock­cooling of the evaporating flask or other glass components
Damage or hazards attributable to use of the product other than as intended are en­
tirely at the risk of the user alone.
Operation Manual Rotavapor® R­100
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2 | Safety
BÜCHI Labortechnik AG
2.3
Staff qualification
Unqualified persons are unable to identify risks and are therefore exposed to greater
dangers.
The device may only be operated by suitably qualified laboratory staff.
These operating instructions are aimed at the following target groups:
Users
Users are persons that meet the following criteria:
— They have been instructed in the use of the device.
— They are familiar with the contents of these operating instructions and the applica­
ble 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 as­
pects:
— 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 hazard­conscious working practices.
— Safety­related 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
Residual risks
The device has been developed and manufactured using the latest technological ad­
vances. 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.
2.4.1
Dangerous vapors
Distillation can produce dangerous vapors that are capable of causing life­threatening
toxic effects.
Do not inhale any vapors produced during distillation.
Ensure that vapors are removed immediately by a suitable fume hood.
Only use the device in well ventilated areas.
If vapors escape from joints or connections, check the seals concerned and re­
place them if necessary.
u Do not distill any unknown fluids.
u Observe the safety data sheets for all fluids used.
u
u
u
u
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2.4.2
Safety | 2
High internal pressure
The evaporation of fluids can produce high pressures inside the flask or the con­
denser. If that pressure becomes too great, the glass components could explode.
u Make sure that the internal pressure inside the glass components is never greater
than atmospheric pressure.
u When distilling without a vacuum, set the vacuum pump to atmospheric pressure
so that excess pressure is automatically dissipated.
u If a vacuum pump is not used, leave the vacuum connection open.
2.4.3
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.
2.4.4
Glass breakage
Broken glass can cause severe cuts.
Damaged glass components may implode if subjected to a vacuum.
Minor damage to the ground joints impairs the sealing effect and may therefore reduce
diminish distillation capacity.
u Handle the flask and other glass components carefully and do not drop them.
u Always place the flasks in a suitable holder when they are not mounted on the Ro­
tavapor.
u Always visually inspect glass components for damage every time they are to be
used.
u Do not continue to use glass components that are damaged.
u Always wear protective gloves when disposing of broken glass.
2.4.5
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 ro­
tating parts.
At high speeds, the heating fluid may be sprayed out by the rotation of the evaporating
flask.
u
u
u
u
u
2.4.6
Wear work overalls or protective clothing.
Do not wear loose or baggy items of clothing such as scarves or neck­ties.
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 or exposed electrical wires can cause injuries.
u Regularly check device for visible damage.
u If faults occur, switch off the device immediately, unplug the power cord and inform
the operator.
u Do not continue to use devices that are damaged.
2.5
Personal protective equipment
Depending on the application, hazards due to heat and/or corrosive chemicals may
arise.
Operation Manual Rotavapor® R­100
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2 | Safety
BÜCHI Labortechnik AG
u Always wear appropriate personal protective equipment such as safety goggles,
protective clothing and gloves.
u Make sure that the personal protective equipment meets the requirements of the
safety data sheets for all chemicals used.
2.6
Modifications
Unauthorized modifications may impair safety and lead to accidents.
u Use only genuine BUCHI accessories, spare parts and consumables.
u 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.
BUCHI accepts no liability whatsoever for damage arising as a result of unauthorized
modifications.
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Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
Product description | 3
3
Product description
3.1
Description of function
The Rotavapor® R­100 is a rotary evaporator with the aid of which single­stage distil­
lation can be carried out quickly without unduly stressing the product. The basis of the
process is the evaporation and condensing of solvents using a rotating evaporating
flask under vacuum. Distillation under vacuum increases capacity and is more gentle
on the product.
The product is heated in the evaporating flask by the heating bath. The rotary drive
unit evenly rotates the evaporating flask. This constantly mixes the product, thereby
increasing the evaporation rate. Rotation also prevents localized overheating and de­
layed evaporation.
The vapor passes from the evaporating flask through the vapor duct into the cooling
section (condenser). There, the thermal energy of the vapor is transferred to the
coolant fluid so that the vapor re­condenses. The resulting solvent is collected in the
receiving flask and can then be reused or properly disposed of.
Distillation under vacuum
The distillation capacity depends on the temperature of the heating bath, the pressure
in the evaporating flask, the speed of rotation and the size of the evaporating flask.
Lower pressure, i.e. more vacuum, reduces the boiling point of the solvent so that it
requires less heating. That means that it can be distilled more gently and at a faster
evaporation rate than processes carried out under normal ambient conditions.
To prevent undesirable solvent emission and delayed evaporation, the vacuum has to
be adjusted to suit the application and kept stable. This can be achieved by means of
a vacuum pump (we recommend the BUCHI Vacuum Pump V­100) controlled by a
vacuum regulator (we recommend the BUCHI Interface I­100). We also recommend
that the temperature difference between the coolant fluid and the heating bath is 40 °C
(see Chapter 6.2.2 "Adjusting distillation conditions", page 34).
Operation Manual Rotavapor® R­100
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3 | Product description
BÜCHI Labortechnik AG
3.2
Configuration
3.2.1
Front view
13
Fig. 1: Configuration of R­100 with V­condenser
1 Condenser
9 Rotary drive unit
2 Glass stopcock
10 Combi­clip
3 Solvent feeding
11 Evaporating flask
4 Power supply for rotary drive unit
12 Heating bath
5 Receiving flask
13 Master switch
6 Handle for height adjustment
7 Lower vertical stop
8 Vertical operating range adjuster
Fig. 2: Rotary drive unit
12/60
1 Rotation speed control
3 Rotary drive locking button
2 Immersion angle locking lever
4 Combi­clip
Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
3.2.2
Product description | 3
Rear view
Fig. 3: Rear view R­100
1 Power supply connection
3 Vacuum connection
2 Fuse
4 Coolant fluid connection
5 Power supply for rotary drive unit
3.2.3
Heating bath user interface
4
Fig. 4: Heating bath user interface
1 Temperature display
3 Master switch
2 Heating process indicator (dot)
4 Adjustment buttons
Operation Manual Rotavapor® R­100
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3 | Product description
3.2.4
BÜCHI Labortechnik AG
Typical application
In order to use the Rotavapor® R­100 to best effect, we recommend that it is used to­
gether with the following peripheral devices:
Recirculating
Chiller F-100
Fig. 5: Rotavapor® R­100 system
1 Recirculating Chiller F­100/F­105
2 Rotavapor® R­100
3 Vacuum Pump V­100 with Interface I­100
The Vacuum Pump V­100 is designed for evacuating laboratory apparatus with the aid
of a PTFE membrane. It can be operated either as a standalone device or combined
with optional accessories such as an interface unit and a secondary condenser to form
a complete vacuum system.
The F­100 and F­105 are sealed­system recirculating chillers. They are available in
various capacity ratings.
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Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
3.2.5
Product description | 3
Type plate
The type plate is on the right­hand side of the Rotavapor® R­100.
BUCHI Operations India Pvt Ltd
394230 Surat / India
Type: R-100
SN:
1000000000
Volt:
100 – 240 VAC
Frequ.: 50/60 Hz
Power: 210 W
Built:
2014
Designed by BUCHI in Switzerland,
Made in India
1
2
3
4
5
6
7
8
9
11
10
Fig. 6: Type plate (example)
1 Company name and address
7 Year of manufacture
2 Device name
8 Country of manufacture
3 Serial number
9 Approvals
4 Input voltage
10 Symbol for "Do not dispose of as
household waste"
5 Frequency
11 Product code
6 Maximum power rating
Operation Manual Rotavapor® R­100
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3 | Product description
BÜCHI Labortechnik AG
3.2.6
Warning symbols on the device
The device carries the following warning symbol:
3.3
Specifications supplied
System with glassware System without glass­
ware
Rotavapor® R­100
1
1
Heating bath B­100
1
1
Condenser (as per order number)
1
–
Vapor duct (with combi­clip)
1
–
Vacuum seal (KD22)
1
1
Evaporating flask (1 litre)
1
–
Receiving flask (1 litre)
1
–
Solvents table flyer
1
1
1 set
–
1
1
Required coolant and vacuum
tubing
Power cord
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Product description | 3
3.4
Technical data
3.4.1
Rotavapor® R­100
3.4.2
Dimensions (W x H x D)
617 x 898 x 502 mm (inc. condenser and heating
bath)
480 x 626 x 502 mm (w/o condenser and heating
bath)
Weight
18 – 19 kg (depending on glassware included)
Voltage
24 V DC
Power consumption
30 W
Enclosure rating
IP21
Immersion angle
0 – 35°
Adjustable height
150 mm (+ 100 mm optional extension)
Rotation speed
20 – 280 rpm
Flask size
50 – 4000 mL
Max. flask capacity
3 kg
Approval
CE
Heating bath B­100
Dimensions (W x H x D)
285 x 219 x 326 mm
Weight
3.9 kg
Voltage
100 – 120 V/220 – 240 V
Frequency
50 – 60 Hz
Power consumption
1700 W
Heater output
1300 W
Enclosure rating
IP21
Fuse
T 12.5 A L 250 V (100 – 120 V)
T 6.3 A L 250 V (220 – 240 V)
Temperature range
20 – 95 °C
Max. flask size
4000 mL
Adjustment accuracy
± 1 %
Bath capacity
4 L
High temperature cut­out
> 145 °C
Approval
CE
Operation Manual Rotavapor® R­100
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3 | Product description
3.4.3
BÜCHI Labortechnik AG
Ambient conditions
Max. altitude above sea level
2000 m
Ambient temperature
10 – 40 °C
Maximum relative humidity
80 % for temperatures up to 31 °C
decreasing linearly to 50 % at 40 °C
The Rotavapor® may only be used in indoor areas.
3.4.4
18/60
Materials
Component
Material
Rotavapor housing
Anodized aluminium with powder coating
Heating bath housing
PBT, partially glass­fiber reinforced
Heating bath
Stainless steel 1.4404, glass­peened
Safety guard
Polycarbonate
Guard ring (of safety guard)
PBT, partially glass­fiber reinforced
Rotary drive unit
Stainless steel 1.4305
Flange connection to condenser
Aluminium
Seal
NBR, PTFE
Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
Product description | 3
3.5
Safety features
3.5.1
Overheat cut­out
To protect against overheating, the heating bath has a thermostatic bath temperature
control.
In addition it is fitted with an electronic and a mechanical overheat cut­out.
The electronic overheat cut­out monitors the temperature limit (the actual temperature
of the bath must not exceed the specified temperature by more than 2 °C for longer
than 2 minutes) the heating rate ( the actual temperature must not increase by more
than 5 °C within 5 seconds) and the function of the temperature sensor. If the elec­
tronic overheat cut­out trips, the device should be inspected by a BUCHI service tech­
nician.
The mechanical overheat cut­out consists of a bi­metallic thermostat that immediately
cuts off the power supply at high temperatures (above 145 °C). The mechanical over­
heat cut­out has to be manually reset once the heating bath has cooled down (see
Chapter 8.2.1 "Resetting overheat safety cut­out", page 44).
3.5.2
Protection against electrical overload
The heating bath is equipped with fuses to protect against electrical overload.
The rotary drive unit has an electrical overload cut­out.
3.5.3
Clips and holders
— Combi­clips 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
3.5.4
Glassware
— High­quality borosilicate glass 3.3
— GL14 hose barbs for preventing glass breakage
3.5.5
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
(see Chapter 10.2 "Spare parts and accessories", page 48)
Operation Manual Rotavapor® R­100
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4 | Transport and storage
BÜCHI Labortechnik AG
4
Transport and storage
4.1
Transport
IMPORTANT
Risk of breakage due to incorrect transportation
u Make sure that the device is fully dismantled and all parts of the device are safely
packed in such a way as to prevent breakage, ideally in the original box.
u Avoid sharp movements during transit.
u After transportation, check the device and all glass components for damage.
u Damage that has occurred in transit should be reported to the carrier.
u Keep packing for future transportation.
4.2
Storage
u Make sure that the ambient conditions are complied with (see Chapter 3.4 "Techni­
cal data", page 17).
u Wherever possible, store the device in its original packaging.
u After storage, check the device, all glass components, seals and tubing for damage
and replace if necessary.
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Installation | 5
5
Installation
5.1
Installation site
The installation site must meet the following requirements:
— Firm and level surface
— Space requirements: at least 620 mm x 510 mm (W x D)
— If distilling under vacuum, there must be a fume hood available.
Wherever possible, the Rotavapor® R­100 should be set up inside the fume hood.
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
Mounting the rotary drive unit
IMPORTANT
Risk of property damage due to rotary drive unit falling off
u Make sure that the screw for fixing the rotary drive unit engages securely in the
groove in the tower mount.
u Slide rotary drive unit (2) onto the tower mount (1).
u Tighten screw (4) to lock the rotary drive unit in the groove (3) so that it cannot be
pulled off.
u Tighten the locking lever (5) for the immersion angle.
u Check that the rotary drive unit cannot be pulled off or twisted.
Operation Manual Rotavapor® R­100
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5 | Installation
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5.3
Fitting the vapor duct and condenser
1
2
2
3
4
u Insert vapor duct (4) into the rotary drive unit.
The vapor duct snaps into place with an audible click.
u NOTICE! Risk of seal damage if fitted incorrectly. Insert seal (2) into the flange
of the condenser (1) as shown.
u Fit condenser (1) into the rotary drive unit, keeping it straight as you do so. When
doing so, make sure that the inner lip of the seal (2) does not fold over as the seal
would then be destroyed.
u Tighten the cap nut (3) to fix the condenser in position. When doing so, make sure
that the spring clip in the cap nut completely encircles the neck of the condenser.
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Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
5.4
Installation | 5
Fitting the glass stopcock
Materials required:
— Grease Glisseal 40 blue (order number 048197)
u Connect a supply tubing for solvent (2).
u Apply a thin coat of Grease Glisseal 40 blue to the glass stopcock (1).
u Insert glass stopcock into the condenser and turn to the desired position.
The glass stopcock performs various functions depending on its position:
— Glass stopcock handle pointing forwards or backwards: the system is sealed. This
is the standard position for distillation.
— Glass stopcock handle pointing upwards: system is being vented.
— Glass stopcock handle pointing downwards: additional solvent can be fed into the
evaporating flask via a connected feeding tubing.
Operation Manual Rotavapor® R­100
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5 | Installation
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5.5
Connecting the vacuum and cooling media tubing
To achieve optimum distillation, all devices in the system should be matched to one
another. Therefore, we recommend that the Rotavapor® R­100 is used together with
the BUCHI Vacuum Pump V­100 and the BUCHI Recirculating Chiller F­100 or F­105
(see Chapter 3.2.4 "Typical application", page 14).
u Connect cooling media tubes to the two coolant connections (2) and (3) using
GL14 cap nuts. There is no need to distinguish between flow and return when do­
ing so.
u Connect the vacuum tubing to the vacuum connection (1) using a GL14 cap nuts.
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Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
5.6
Installation | 5
Electrical connections
u Make sure that the available power supply matches the rating indicated on the type
plate.
u Plug the rotary drive unit connecting lead into the socket (2) on the heating bath.
u Plug the power cord into the socket (1) on the heating bath and then into a mains
power socket.
u If an extension lead is required, make sure that it is earthed and has a suitable
power rating.
5.7
Overview of connections
The diagram below shows the connection of tubing and electrical leads in a typical ap­
plication of the Rotavapor® R­100 in conjunction with a Recirculating Chiller F­105, a
Vacuum Pump V­100, an Interface I­100 and a Woulff bottle (see also Chapter 3.2.4
"Typical application", page 14).
IN
OUT
The connections to the Recirculating Chiller F­105, the Vacuum Pump V­100 and the
Interface I­100 are described in the particular operating instructions in each case.
Operation Manual Rotavapor® R­100
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5 | Installation
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5.8
Setting up and filling the heating bath
1
2
u Locate the heating bath (1) in the L­shaped cut­out in the Rotavapor base (2).
IMPORTANT
Risk of heating bath corrosion due to use of unsuitable heating fluid
u Do not use pure distilled water or de­ionised water.
u If pure distilled or de­ionised water has to be used, add 1 to 2 g of Borax (Na2B4O7
x 10 H2O) per litre of water.
The recommended fluid for use in the heating bath is water. Normal tap water may be
mixed with distilled water with a mixing ratio of up to 1:1 according to the water hard­
ness.
u Fill the heating bath with suitable fluid.
5.9
Quick check
u To complete the installation process, check the following points:
u Switch on the rotary drive unit, change the rotation speed and check that the evap­
orating flask rotates at a different speed.
u 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 (Chapter 6.1.1 "Prepar­
ing the heating bath", page 27).
u Check that the height of the rotary drive unit can be adjusted (see Chapter 6.1.5
"Vertical adjustment", page 30).
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Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
Operation | 6
6
Operation
6.1
Preparations
6.1.1
Preparing the heating bath
CAUTION
Risk of skin burns from hot fluids and surfaces
u Do not put your hands in the hot fluid.
u Do not carry, shift, tip or otherwise move the heating bath when it is filled with hot
fluid.
u Do not fill the heating bath right to the very top. Allow for the expansion of the fluid
when heated.
u Do not switch on the heating bath when it is empty.
CAUTION
Using oil as a heating fluid
Risk of skin burns from oil splashes
u Never pour water into hot oil.
u Make sure that the oil used is suitable for these purposes.
4
u Make sure that the heating bath is filled.
u Switch on the device at the master switch (3).
The heating bath temperature last set is displayed.
u Set the desired temperature using the adjustment buttons (4).
The set temperature (1) flashes during adjustment. Afterwards, the current actual
temperature is indicated and the heater switched on.
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6 | Operation
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6.1.2
Fitting the evaporating flask
IMPORTANT
Risk of evaporating flask damage if fitted incorrectly
u When fitting the evaporating flask make sure that the edge of the glass does not
strike the vapor duct.
u Tighten combi­clip no more than hand­tight.
u Carefully fit evaporating flask (3) onto the vapor duct (2).
u Slide clip (4) over the neck of the flask.
u Screw combi­clip (1) clockwise until hand­tight.
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Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
6.1.3
Operation | 6
Adjusting immersion angle of evaporating flask
u Switch off the Rotavapor on the heating bath.
u Hold the condenser (1) firmly with one hand and release the lever (2) with the other
hand.
u Adjust the immersion angle.
u Lock the rotary drive unit in position again with the lever (2).
u Make sure that there is at least 10 mm clearance between the edge of the heating
bath and the evaporating flask or vapor duct. To achieve that, adjust the height of
the rotary drive unit if necessary (see Chapter 6.2.1 "Raising and lowering the
evaporating flask", page 33).
u Check the vertical end stop and adjust if necessary (see Chapter 6.1.5 "Vertical ad­
justment", page 30).
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6 | Operation
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6.1.4
Fitting the receiving flask
Materials required:
— Grease Glisseal 40 blue (order number 048197)
u Apply a thin coat of Grease Glisseal 40 blue to the ground joint of the receiving
flask.
u Fit the receiving flask (3) onto the condenser from below and secure it with the ball
joint clamp (2).
6.1.5
Vertical adjustment
1
2
3
The rotary drive unit together with the glass components can be raised or lowered in
the following ways:
— Using the handle (1), the evaporating flask can be lowered into and lifted out of the
heating bath (see Chapter 6.2.1 "Raising and lowering the evaporating flask", page­
33). To prevent the evaporating flask and the vapor duct from colliding with the
heating bath, a lower stop can be set using the screw­handle (2).
— If an especially large evaporating flask or a long vapor duct is being used, the entire
vertical adjustment range can be moved up or down by means of screw­handle (3)
(see Chapter "Moving the vertical adjustment range up/down", page 31).
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Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
Operation | 6
Moving the vertical adjustment range up/down
CAUTION
Risk of injury when adjusting apparatus height
u Make sure that your fingers are not trapped when adjusting the apparatus height.
u Make sure that all tubing are long enough and are not under strain after making the
adjustment.
1
2
3
u Loosen the two screw­handles (2) and (3).
u Move the rotary drive unit together with the glass components and screw­handles
so that the adjustment range of handle (1) is sufficient to be able to immerse the
evaporating flask in the heating bath and completely lift it out of the heating bath.
u Tighten screw­handle (3).
u Adjust screw­handle (2) so that it acts as a stop for downward adjustment of han­
dle (1). When the handle is at its lowest position, there should be a minimum clear­
ance of 10 mm between the evaporating flask and the edge and/or the bottom of
the heating bath in order to prevent the flask colliding with the heating bath.
>10 mm
u Tighten screw­handle (2).
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6 | Operation
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6.2
Performing distillation
DANGER
Risk of poisoning from inhalation of hazardous vapors
Do not inhale any vapors produced during distillation.
Ensure that vapors are removed immediately by a suitable fume hood.
Only use the device in well ventilated areas.
If vapors escape from joints or connections, check the seals concerned and re­
place them if necessary.
u Do not distill any unknown fluids.
u Observe the safety data sheets for all fluids used.
u
u
u
u
DANGER
Explosion risk from distillation of hazardous materials
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.
WARNING
Risk of explosion from excessive internal pressure
The evaporating flask and/or the condenser could explode if the internal pressure pro­
duced by evaporation becomes too great.
u Make sure that the internal pressure inside the glass components 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.
To achieve optimum distillation results, the following procedure is recommended:
u Adjust the flow rate of the coolant to suit the type of coolant and the cooling capac­
ity. If tap water is used, the flow rate should be at least 40 L/h.
u Make sure that the coolant temperature is not more than 20 °C.
u Pour solvent into evaporating flask and fit evaporating flask (see Chapter 6.1.2 "Fit­
u
u
u
u
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ting the evaporating flask", page 28).
Make sure that the receiving flask is fitted.
Close the glass stopcock.
Switch on the rotary drive unit and adjust the rotation speed if necessary.
Set the vacuum so that the boiling point of the solvent is 20 °C below the tempera­
ture of the heating bath.
Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
Operation | 6
u Immerse the evaporating flask in the heating bath (see Chapter 6.2.1 "Raising and
lowering the evaporating flask", page 33).
u Wait 1 – 2 minutes to make sure distillation starts.
u If necessary, adjust the vacuum and/or the heater temperature (see Chapter 6.2.3
"Optimization distillation", page 35).
6.2.1
Raising and lowering the evaporating flask
CAUTION
Risk of scalding if heating bath overflows
u When immersing the evaporating flask, make sure that the fluid does not overflow
due to the displacement.
u When the evaporating flask is rotating look out for splashing fluid.
CAUTION
Risk of injury when adjusting apparatus height
u Make sure that your fingers are not trapped when adjusting the apparatus height.
u Make sure that all tubing are long enough and are not under strain after making the
adjustment.
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.
u Press and hold down the vertical adjustment handle release button (2).
u Move the rotary drive unit up or down by means of the vertical adjustment handle
(1).
u Let go of the release button to lock the handle at the desired height.
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6 | Operation
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6.2.2
Adjusting distillation conditions
To obtain optimum distillation conditions, the energy absorbed by the solvent from the
heating bath must be removed again in the condenser. To achieve that, the following
settings are recommended:
20 °C 1
Δ
20 °C
40 °C 2
Δ
20 °C
60 °C 3
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 condenser should be 20 °C in each case.
The pressure in the evaporating flask should be set so that the boiling point of the sol­
vent is around 40 °C (see Chapter 10.1 "Solvent table", page 47).
The flow rate of the coolant depends on the type of coolant used and the capacity of
the cooler but should be at least 40 – 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.
To achieve optimum distillation, all devices in the system should be matched to one
another. Therefore, we recommend that the Rotavapor® R­100 is used together with
the BUCHI Vacuum Pump V­100 and the BUCHI Recirculating Chiller F­105 (see
Chapter 3.2.4 "Typical application", page 14). That will enable achievement of a stable
vacuum and stable cooling, and thus a more efficient distillation process.
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Operation Manual Rotavapor® R­100
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6.2.3
Operation | 6
Optimization distillation
Depending on the solvent involved, it may also be possible to further optimize the dis­
tillation process. The distillation should always be set up so that the condensate does
not cover more than three quarters of the coil in the condenser. The top quarter should
remain exposed.
WARNING
Risk of explosion from excessive internal pressure
The evaporating flask and/or the condenser could explode if the internal pressure pro­
duced by evaporation becomes too great.
u Make sure that the internal pressure inside the glass components is never greater
than atmospheric pressure.
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.
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.
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6 | Operation
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u In applications where no vacuum is applied, lower the temperature of the heating
bath.
That will cause less solvent to evaporate.
6.2.4
Feeding solvent during distillation
Precondition:
R An external vacuum pump is connected and running.
R A feed tubing leading from the glass stopcock to the evaporating flask is fitted.
u Connect a supply tubing (2) for the solvent to the glass stopcock (1) and hold it in
the solvent.
u Turn the glass stopcock until the handle is pointing downwards.
Solvent is drawn into the evaporating flask by the vacuum.
u Make sure that there is not more than 3 kg of solvent in the evaporating flask.
u Close the glass stopcock.
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Operation Manual Rotavapor® R­100
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6.3
Operation | 6
Finishing distillation
u Raise the rotary drive unit (see Chapter 6.2.1 "Raising and lowering the evaporat­
u
u
u
u
u
u
u
u
u
6.3.1
ing flask", page 33).
Vent the Rotavapor.
Turn off the rotary drive unit (set the rotation speed to 0 rpm).
Switch off the heating bath
CAUTION! Risk of skin burns from hot evaporating flask. Check the tempera­
ture of the evaporating flask and, if necessary, allow it to cool down or else wear
suitable protective gloves.
Remove the evaporating flask (see Chapter 6.3.1 "Removing the evaporating
flask", page 37).
Turn off the coolant supply.
Remove the receiving flask (see Chapter 6.3.2 "Removing the receiving flask",
page 38).
Dry the Rotavapor (see Chapter 7.6 "Removing solvent accumulations", page 41).
Clean the Rotavapor and all glass components (see Chapter 7 "Cleaning and ser­
vicing", page 39).
Removing the evaporating flask
1
3
4
u Raise the rotary drive unit (see Chapter 6.2.1 "Raising and lowering the evaporat­
ing flask", page 33).
u Vent the Rotavapor.
u Turn off the rotary drive unit (set the rotation speed to 0 rpm).
u CAUTION! Risk of skin burns from hot evaporating flask. Check the tempera­
u
u
u
u
ture of the evaporating flask and, if necessary, allow it to cool down or else wear
suitable protective gloves.
Firmly hold the evaporating flask (4) and release the combi­clip (3) by screwing it
counter­clockwise.
Push the clip (2) back from the neck of the evaporating flask.
Detach the evaporating flask.
If the evaporating flask sticks because of chemical residues, press the lock release
button (1) and twist the flask (4) counter­clockwise to remove it.
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6.3.2
Removing the receiving flask
u Raise the rotary drive unit (see Chapter 6.2.1 "Raising and lowering the evaporat­
ing flask", page 33).
u Vent the Rotavapor.
u Turn off the rotary drive unit (set the rotation speed to 0 rpm).
u Firmly hold the receiving flask (3), remove the ball joint clamp (2) and remove the
receiving flask.
u Make sure that any dripping condensate cannot cause any damage.
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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 sec­
tion.
Any servicing and repair work which involves opening up the housing may only be
carried out by BUCHI service technicians.
u Use only genuine BUCHI consumables and spare parts in order to ensure correct
operation of the device and preserve the warranty.
u .
7.1
Inspecting and cleaning the vapor duct
1
2
u Switch off the device.
u Remove the evaporating flask (see Chapter 6.3.1 "Removing the evaporating
flask", page 37).
u Press the lock release button (1) on the front of the rotary drive unit.
u Firmly hold the vapor duct and turn the combi­clip (2) clockwise until the vapor duct
is released.
u Visually inspect the vapor duct for damage, wear marks and residues.
u Clean the vapor duct with a paper towel and water or ethanol.
u Refit the vapor duct (see Chapter 5.3 "Fitting the vapor duct and condenser", page­
22).
7.2
Checking the system for leaks
Precondition:
R An external vacuum pump with a pressure gauge is connected.
u Make sure that all flasks are fitted and the glass stopcock is closed.
u Connect the vacuum pump and evacuate the R­100 to a pressure of 50 mbar.
u 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.
u Check the pressure after one minute.
5 If the pressure has risen by less than 3 mbar after one minute, the system is air­
tight.
If the system is not air­tight:
u Check all seals (see Chapter 7.3 "Checking seals", page 40).
u Examine all tubing and replace if they are brittle or cracked.
u Grease ground glass joints if necessary.
Operation Manual Rotavapor® R­100
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7 | Cleaning and servicing
7.3
BÜCHI Labortechnik AG
Checking seals
Seals are wear parts. They have to be regularly inspected, cleaned and, if necessary,
replaced. The life of a seal depends on much it is used and how well it is looked after.
1
2 3
4
5
1 Vacuum connection seal
4 Feed tubing seal
2 Coolant seal
5 Vacuum gasket (not visible)
3 Coolant seal
u Remove seals and inspect for damage and cracks.
u Rinse intact seals in water or ethanol and dry with a soft cloth.
u Replace damaged seals and check the corresponding glass contact faces for dam­
age (e.g. wear marks).
NOTE
New PTFE seals require approx. 10 hours to achieve an optimum seal.
7.4
Cleaning the condenser
u Using a wash bottle, squirt ethanol into the vacuum connection of the condenser
and rinse it out.
u After rinsing allow the ethanol to drain out at the bottom.
u Use an alkaline cleaning agent to remove stubborn dirt (e.g. algae).
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7.5
Cleaning and servicing | 7
Cleaning the heating bath
IMPORTANT
Risk of short circuit from fluid penetration into device
u Do not immerse heating bath or rotary drive unit in water or pour water over them.
u Only wipe down the housing with a damp cloth.
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 stainless steel surface of the heating bath starts to rust
u Unplug the power supply for the heating bath and rotary drive unit.
u Allow the heating bath to cool down then empty it.
u Remove small amounts of limescale in the bowl of the heating bath using non­
abrasive cleaners (e.g. household cleaner and washing­up sponge).
u Use acetic acid to dissolve stubborn limescale deposits. Afterwards thoroughly
rinse out the bath.
7.6
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 Fit a clean and dry evaporating flask and receiving flask (see Chapter 6.1.2 "Fitting
u
u
u
u
u
u
the evaporating flask", page 28 and Chapter 6.1.4 "Fitting the receiving flask",
page 30).
Make sure that the glass stopcock is closed.
Connect the vacuum pump and evacuate the R­100 as much as possible.
Allow the vacuum pump to run for a further 2 to 3 minutes.
Vent the Rotavapor.
Check that all solvent accumulations have been removed.
Dispose of solvent residues in accordance with the specifications of the applicable
safety data sheet.
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8 | Help with faults
BÜCHI Labortechnik AG
8
Help with faults
8.1
Faults, possible causes and remedies
Fault
Possible cause
Remedy
Device does not
work
Device is not connected to
power supply
u Check power supply (see
Fuse blown
u Replace fuse (see Chapter­
Chapter 5.6 "Electrical con­
nections", page 25).
8.2.2 "Replacing the fuse",
page 45).
u If fault recurs, contact
BUCHI Customer Service.
Heating bath
fails to heat up
Device is not connected to
power supply
u Check power supply (see
High temperature cut­out has
tripped
u Reset the overheat safety
Fuse blown
u Replace fuse (see Chapter­
Chapter 5.6 "Electrical con­
nections", page 25).
cut­out (see Chapter 8.2.1
"Resetting overheat safety
cut­out", page 44).
8.2.2 "Replacing the fuse",
page 45).
u If fault recurs, contact
BUCHI Customer Service.
System leaking
Ground glass joints not greased u Grease ground glass joints.
Tubing leaking
u Replace tubing (see Chap­
ter 5.5 "Connecting the vac­
uum and cooling media tub­
ing", page 24).
Seal defective
u Replace seal (see Chapter­
7.3 "Checking seals", page­
40).
Vacuum is not
achieved
Back­evaporation from the re­
ceiving flask
u Empty the receiving flask
Temperature difference be­
tween evaporating flask and
condenser less than 20 °C
u Increase cooling (see Chap­
System leaking
u Check system for leaks (see
(see Chapter 6.3.2 "Remov­
ing the receiving flask",
page 38).
ter 6.2.2 "Adjusting distilla­
tion conditions", page 34).
Chapter 7.2 "Checking the
system for leaks", page 39).
Water pressure of glass filter
pump too low
u Increase water flow (see
Vacuum pump too weak
u Use suitably dimensioned
pump operating instructions).
vacuum pump.
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Help with faults | 8
Fault
Possible cause
Optimum distilla­ Too much back­evaporation
tion not
from the receiving flask (espe­
achieved
cially with solvent mixtures)
Other faults in distillation
process (e.g. sudden cooling,
too little heat flow, etc.)
Operation Manual Rotavapor® R­100
Remedy
u Empty receiving flask and
restart distillation (see Chap­
ter 6.3.2 "Removing the re­
ceiving flask", page 38,
Chapter 6.1.4 "Fitting the re­
ceiving flask", page 30 and
Chapter 6.2 "Performing dis­
tillation", page 32).
u Check temperatures of heat­
ing bath and coolant and ad­
just as necessary (see
Chapter 6.1.1 "Preparing the
heating bath", page 27 and/
or cooler operating instruc­
tions).
u Lower pressure until distilla­
tion resumes (see vacuum
pump operating instructions).
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8 | Help with faults
BÜCHI Labortechnik AG
8.2
Remedy
8.2.1
Resetting overheat safety cut­out
CAUTION
Risk of skin burns from hot components
u Do not touch hot components unless wearing suitable protective gloves.
u
u
u
u
Switch off the device.
Unplug the power supply for the heating bath and rotary drive unit.
Allow the heating bath to cool down then empty it.
Using a narrow object or screwdriver, press the switch (1) on the underside of the
heating bath.
5 The overheat safety cut­out is reset.
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8.2.2
Help with faults | 8
Replacing the fuse
The fuse is on the rear of the heating bath.
u
u
u
u
u
u
Allow the heating bath to cool down.
Disconnect the power cord.
Open the fuse holder (1) with a large screwdriver.
Replace the blown fuse with an intact one of the same rating.
Screw the fuse holder (1) back in.
Reconnect the power cord.
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9 | Taking out of service and disposal
BÜCHI Labortechnik AG
9
Taking out of service and disposal
9.1
Taking out of service
u Remove all fluids from the glass components (see Chapter 7.6 "Removing solvent
accumulations", page 41).
u Switch off the device.
u Unplug the power supply for the heating bath and rotary drive unit.
u Remove all glass components.
9.2
Disposal
The operator is responsible for proper disposal of the Rotavapor®.
u When disposing of equipment observe the local regulations and statutory require­
ments regarding waste disposal.
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Appendix | 10
10
Appendix
10.1
Solvent table
Solvent
Formula
Molar
Evaporation en­ Boiling
mass in g/ ergy in J/g
point in °C
mol
at 1013
mbar
Density in Vacuum in
g/cm3
mbar for 40­
°C boiling
point
Acetone
CH3H6O
58.1
553
56
0.790
556
n­Amyl alcohol, n­pentanol
C5H12O
88.1
595
37
0.814
11
Benzene
C 6H 6
78.1
548
80
0.877
236
n­butanol
C4H10O
74.1
620
118
0.810
25
Tert butyl alcohol (2­ C4H10O
methyl­2­propanol)
74.1
590
82
0.789
130
Chlorobenzene
C6H5Cl
112.6
377
132
1.106
36
Chloroform
CHCl3
119.4
264
62
1.483
474
Cyclohexane
C6H12
84.0
389
81
0.779
235
Diethyl ether
C4H10O
74.0
389
35
0.714
850
1,2­dichloroethane
C2H4Cl2
99.0
335
84
1.235
210
cis­1,2­dichloroethy­ C2H2Cl2
lene
97.0
322
60
1.284
479
trans­1,2­
dichloroethylene
C2H2Cl2
97.0
314
48
1.257
751
Di­isopropyl ether
C6H14O
102.0
318
68
0.724
375
Dioxane
C4H8O2
88.1
406
101
1.034
107
DMF (dimethylfor­
mamide)
C3H7NO
73.1
–
153
0.949
11
Acetic acid
C2H4O2
60.0
695
118
1.049
44
Ethanol
C 2H 6O
46.0
879
79
0.789
175
Ethylacetate
C4H8O2
88.1
394
77
0.900
240
Heptane
C7H16
100.2
373
98
0.684
120
Hexane
C6H14
86.2
368
69
0.660
360
Isopropylalcohol
C 3H 8O
60.1
699
82
0.786
137
Isoamylalcohol (3­
methyl­1­butanol)
C5H12O
88.1
595
129
0.809
14
Methylethylketone
C 4H 8O
72.1
473
80
0.805
243
Methanol
CH4O
32.0
1227
65
0.791
337
Methylene chloride,
dichloromethane
CH2CI2
84.9
373
40
1.327
850
Pentane
C5H12
72.1
381
36
0.626
850
n­propylalcohol
C 3H 8O
60.1
787
97
0.804
67
Pentachloroethane
C2HCl5
202.3
201
162
1.680
13
Operation Manual Rotavapor® R­100
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10 | Appendix
BÜCHI Labortechnik AG
Solvent
Formula
Molar
Evaporation en­ Boiling
mass in g/ ergy in J/g
point in °C
mol
at 1013
mbar
Density in Vacuum in
g/cm3
mbar for 40­
°C boiling
point
1,1,2,2­tetra­
chloroethane
C2H2Cl4
167.9
247
146
1.595
20
Carbon tetrachloride CCl4
153.8
226
77
1.594
271
1,1,1­trichloroethane C2H3Cl3
133.4
251
74
1.339
300
Tetrachloroethylene
C2Cl4
165.8
234
121
1.623
53
THF (tetrahydrofu­
rane)
C 4H 8O
72.1
–
67
0.889
374
Toluene
C 7H 8
92.2
427
111
0.867
77
Trichloroethylene
C2HCl3
131.3
264
87
1.464
183
Water
H 2O
18.0
2261
100
1.000
72
Xylene (mixture)
C8H10
106.2
389
–
–
25
o­xylene
C8H10
106.2
–
144
0.880
–
m­xylene
C8H10
106.2
–
139
0.864
–
p­xylene
C8H10
106.2
–
138
0.861
–
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.
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Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
10.2.1
Appendix | 10
Glass apparatus V
11055921
040627
11055922 P+G
028606
040625
000636
000646
048237
023875
023900
028096
032339 (STJ 29/32)
032341 (STJ 24/40)
003275
Order no.
Description
11057056
Glass assembly V. Vertical condenser,
1460cm²
11055921 Condenser V. Vertical cond., 1460cm²
11057057 Glass condenser V. Vertical cond.,
Order no.
Description
000646
Tubing. PTFE, Ø4.7/5.5mm, transpar­
ent, 330mm
000636
Vacuum gasket. KD22, PTFE
028096
Tubing. PTFE, Ø3/4mm, white, 600mm
1460cm², P+G
038000
Hose barbs, set. 6 pcs., bent (4),
straight (2), GL14, silicone seal
040625
Drain disc. PTFE, Ø5.1/14mm
032341
Vapor duct. For V/C cond., Ø22mm,
SJ24/40, incl. combi­clip
003275
Ball joint clamp. For BJ35/20
032339
Vapor duct. For V/C cond, Ø22mm,
SJ29/32, incl. combi­clip
040627
Glass stopcock. Standard, glass, SJ18.8/38
023875
Screw­cap. GL10
037642
Hose barbs, set. 4 pcs., straight, GL14, silicone seal
023900
O­ring. FPM, Ø3.0/2.7mm
037287
Hose barbs, set. 4 pcs., bent, GL14,
silicone seal, incl. cap nut
Operation Manual Rotavapor® R­100
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10 | Appendix
BÜCHI Labortechnik AG
10.2.2
Glass apparatus C
027479
000672
027462
040628
040641
032013
040627
000646
027344
028606
052892
052891
048237
028096
023875
023900
032339 (STJ 29/32)
032341 (STJ 24/40)
003275
000636
Order no.
Description
Order no.
Description
040640
Glass assembly C. Cold trap, 500cm²
040627
Glass stopcock. Standard, glass, SJ18.8/38
040641
Cold trap mantle. For C condenser
038000
Hose barbs, set. 6 pcs., bent (4),
straight (2), GL14, silicone seal
040645
Condenser C. Cold trap, 500cm²
003275
Ball joint clamp. For BJ35/20
000672
Cold finger. For C condenser
023875
Screw­cap. GL10
027479
Lid. For C condenser, PETP
023900
O­ring. FPM, Ø3.0/2.7mm
027462
Seal, set. For C/CR condenser, PTFE, EPDM
037287
Hose barbs, set. 4 pcs., bent, incl. cap nut, GL14
037642
Hose barbs, set. 4 pcs., straight, GL14, 052893
silicone seal
Condenser holder. For V/C
condenser incl. rubber band
032341
Vapor duct. For V/C condenser, Ø22mm, SJ24/40, incl. combi­clip
032013
Rubber band. To fasten condenser
032339
Vapor duct. For V/C condenser, Ø22mm, SJ29/32, incl. combi­clip
027344
Cross sleeve. To fasten condenser
040628
Glass stopcock. For C condenser, glass
000646
Tubing. PTFE, Ø4.7/5.5mm, transpar­
ent, 330mm
50/60
000636
028096
Vacuum gasket. KD22, PTFE
Tubing. PTFE, Ø3/4mm, white, 600mm
Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
10.2.3
Appendix | 10
Accessories
Heating Bath
Heating Bath B­100. 20­95°C, 220­240V
11061895
Heating power: 1300 W, maximum flask size: 4000 mL Allows adjusting
set temperature and indicates actual temperature digitally
Heating Bath B­100. 20­95°C, 100­120V
11061894
Heating power: 1300 W, maximum flask size: 4000 mL Allows adjusting
set temperature and indicates actual temperature digitally
Accessories for heating bath
Top cover. For Heating Bath B­491, B­100
To safe energy and to minimize water evaporation when not in use
048230
Protective shield. For Heating Bath B­491, B­100
048052
Swimming balls. 450pcs, PP, Ø10mm
036405
To reduce energy consumption of heating bath and for less evaporation
of the heating medium, for temperatures up to 100 °C
Tubing
FEP, Ø6/8mm, transparent, per m
Utilization: Vacuum, cooling media
027900
Natural rubber, Ø6/16mm, red, per m Utilization: Vacuum
017622
Nyflex, PVC­P, Ø8/14mm, transparent, per m Utilization: Vacuum, cooling media
004113
PTFE, Ø4.7/5.5mm, transparent, 330mm
To initate solvent into the evaporating flask during distillation
000646
PTFE, Ø8/10mm, white, per m
Utilization: Vacuum, tubing (industrial Rotavapor)
027277
Silicone rubber, Ø6/9mm, transparent, per m
Utilization: Cooling media
004133
Further accessories
Flask holder. Ring, non­slippery EPDM
Holder for round­botton flasks (50 – 5000 mL)
048618
Flask holders, set. 5pcs, ring, non­slippery EPDM
Holder for round­botton flasks (50 – 5000 mL)
11059916
Cooling water valve. 24VAC
Valve opens cooling water feed during distillation, only used in combi­
nation with a vacuum controller/interface
031356
Lab grease. Glisseal 40 (60g)
To grease the joints in order to increase tightness of the system
048197
Manometer with needle valve. Incl. holder for pump, valve, vacuum 047291
gauge
For manual vacuum adjustment
Power adapter. 24VDC, voltage 100­240V, frequency 50/60Hz
For operation of Rotavapor without heating bath
Operation Manual Rotavapor® R­100
11055312
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10 | Appendix
BÜCHI Labortechnik AG
Water regulation nozzle. Restriction valve, hose clamp, sieve
Used when tap water is applied as vacuum source, to reduce flow­rate
of the water
011606
Water jet pump. Plastic
Used when tap water is applied as the vacuum source
002913
Water jet pump, B­764. Magnetic valve, FFKM, 24V
031358
Simple principle of vacuum generation, without cooling water valve, only
used in combination with a vacuum controller/interface
Water jet pump, B­767. Magnetic valve (2pcs), FFKM, 24V
Simple principle of vacuum generation, with cooling water valve, only
used in combination with a vacuum controller/interface
031357
Glassware
Glass assemblies
Glass assembly C. Cold trap, 500cm2
For the distillation of low­boiling point solvents. No need of cooling liq­
uid. Contents: 1 L receiving flask, ball joint clamp, stopcock, feed tub­
ing. Not included: Evaporating flask, vapor duct, holder
040640
Glass assembly C. Cold trap, 500cm2, P+G
For the distillation of low­boiling point solvents. No need of cooling liq­
uid. Contents: 1 L receiving flask, ball joint clamp, stopcock, feed tub­
ing. Not included: Evaporating flask, vapor duct, holder
040642
Glass assembly V. Vertical condenser, 1460cm2
11057056
For standard application. Used with recirculating chiller or tap water.
Features: No top hole. No connection for vapor temperature sensor.
Contents: 1 L receiving flask, ball joint clamp, stopcock, feed tubing. Not
included: Evaporating flask, vapor duct, holder
Glass assembly V. Vertical condenser, 1460cm2, P+G
11057057
For standard application. Used with recirculating chiller or tap water.
Features: No top hole. No connection for vapor temperature sensor.
Contents: 1 L receiving flask, ball joint clamp, stopcock, feed tubing. Not
included: Evaporating flask, vapor duct, holder
Accessories for glass assemblies
Condenser holder. For V/C­condenser, incl. rubber band
052893
Foam trap adaptor
Glass, Reitmeyer, SJ24/40, 150mm
036577
Glass, Reitmeyer, SJ29/32, 135mm
036576
Glass, bump trap, SJ24/40, 175mm
11056919
Glass, bump trap, SJ29/32, 160mm
11056920
Evaporating flask
52/60
For distillation spider, cylindric, SJ14/23, 20mL
000477
Glass, SJ24/40, 1000mL
000440
Glass, SJ24/40, 1000mL, P+G
020730
Glass, SJ24/40, 100mL
008751
Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
Appendix | 10
Glass, SJ24/40, 2000mL
008765
Glass, SJ24/40, 2000mL, P+G
025262
Glass, SJ24/40, 250mL
008754
Glass, SJ24/40, 3000mL
008767
Glass, SJ24/40, 3000mL, P+G
025263
Glass, SJ24/40, 4000mL
047990
Glass, SJ24/40, 4000mL, P+G
047992
Glass, SJ24/40, 500mL
008758
Glass, SJ24/40, 500mL, P+G
025261
Glass, SJ24/40, 50mL
008750
Glass, SJ29/32, 1000mL
000435
Glass, SJ29/32, 1000mL, P+G
020729
Glass, SJ29/32, 100mL
000432
Glass, SJ29/32, 100mL, P+G
033404
Glass, SJ29/32, 2000mL
000436
Glass, SJ29/32, 2000mL, P+G
025323
Glass, SJ29/32, 250mL
000433
Glass, SJ29/32, 250mL, P+G
025520
Glass, SJ29/32, 3000mL
000437
Glass, SJ29/32, 3000mL, P+G
025324
Glass, SJ29/32, 4000mL
047991
Glass, SJ29/32, 4000mL, P+G
047993
Glass, SJ29/32, 500mL
000434
Glass, SJ29/32, 500mL, P+G
025322
Glass, SJ29/32, 50mL
000431
Glass, SJ29/32, 50mL, P+G
033405
Drying flask
Glass, SJ24/40, 1000mL
000420
Glass, SJ24/40, 2000mL
011580
Glass, SJ24/40, 500mL
011579
Glass, SJ29/32, 1000mL
000453
Glass, SJ29/32, 2000mL
000454
Glass, SJ29/32, 500mL
000452
Beaker flasks
Glass, SJ24/40, 1500mL, for drying
034270
Glass, SJ24/40, 1500mL, for evaporation
034247
Glass, SJ24/40, 500mL, for drying
034768
Glass, SJ24/40, 500mL, for evaporation
034765
Glass, SJ29/32, 1500mL, for drying
034269
Operation Manual Rotavapor® R­100
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10 | Appendix
BÜCHI Labortechnik AG
Glass, SJ29/32, 1500mL, for evaporation
034230
Glass, SJ29/32, 500mL, for drying
034767
Glass, SJ29/32, 500mL, for evaporation
034764
Receiving flasks
Glass, BJ35/20, 1000mL
000425
Glass, BJ35/20, 1000mL, P+G
020728
Glass, BJ35/20, 1000mL, P+G­LT
Application temperature: ­70 to 40 °C
040775
Glass, BJ35/20, 1000mL, P+G, drain valve
036919
Glass, BJ35/20, 100mL
000422
Glass, BJ35/20, 2000mL
000426
Glass, BJ35/20, 2000mL, P+G
025265
Glass, BJ35/20, 2000mL, P+G­LT
Application temperature: ­70 to 40 °C
040776
Glass, BJ35/20, 250mL
000423
Glass, BJ35/20, 250 mL, P+G
11060907
Glass, BJ35/20, 250 mL, P+G­LT
Application temperature: ­70 to 40 °C
11060908
Glass, BJ35/20, 3000mL
000427
Glass, BJ35/20, 3000mL, P+G
025266
Glass, BJ35/20, 3000mL, P+G­LT
Application temperature: ­70 to 40 °C
040777
Glass, BJ35/20, 500mL
000424
Glass, BJ35/20, 500mL, P+G
025264
Glass, BJ35/20, 500mL, P+G­LT
Application temperature: ­70 to 40 °C
040774
Glass, BJ35/20, 50mL
000421
Vapor ducts
For V/C cond., Ø22mm, SJ24/40, incl. Combi­Clip
032341
For V/C cond., Ø22mm, SJ29/32, incl. Combi­Clip
032339
Stopcocks
Stopcock. Professional, glass, SJ18.8/38
For aeration of the system. Less cross­contamination than with stan­
dard­stopcock
000637
Stopcock. PTFE, SJ18.8/38 For aeration of the system. For applications when grease should be
avoided, used instead of standard­stopcock
023896
Stopcock. Standard, glass, SJ18.8/38
For aeration of the system
040627
Distillation spiders
Glass, SJ24/40, incl. 100mL flask (5pcs)
54/60
011575
Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
10.2.4
Appendix | 10
Glass, SJ24/40, incl. 20mL zyl. flask (20pcs)
011578
Glass, SJ24/40, incl. 50mL flask (5pcs)
011574
Glass, SJ29/32, incl. 100mL flask (5pcs)
001333
Glass, SJ29/32, incl. 20mL zyl. flask (12pcs)
001335
Glass, SJ29/32, incl. 20mL zyl. flask (20pcs)
001336
Glass, SJ29/32, incl. 20mL zyl. flask (6pcs)
001334
Glass, SJ29/32, incl. 50mL flask (5pcs)
001332
Wear parts
Vacuum gaskets
KD22, PTFE
000636
KD22, PTFE, FDA­compliant
11056622
Seals
For cap nut, GL14, FEP
038225
Set. 10pcs, for hose barbs, GL14, EPDM, black
040029
Set. 10pcs, for hose barbs, GL14, FPM, green
040040
Set. 20pcs, for hose barbs, GL14, silicone, red
040023
Hose barbs
Bent, GL14, incl. silicone seal
018916
Set. 2pcs, bent (1), straight (1), GL14, silicone seal
Content: Hose barbs, cap nuts, seals
041939
Set. Set. 3pcs, bent, GL14, silicone seal
Content: Hose barbs, seals
041987
Set. 4pcs, bent, GL14, EPDM seal
Content: Hose barbs, cap nuts, seals
043129
Set. 4pcs, bent, GL14, FEP seal
Content: Hose barbs, cap nuts, seals
040295
Set. 4pcs, bent, GL14, silicone seal, incl. cap nut
Content: Hose barbs, cap nuts, seals
037287
Set. 4pcs, bent, GL14, silicone seal, incl. cap nut
Content: Hose barbs, cap nuts, seals
043128
Set. 4pcs, straight, GL14, EPDM seal
Content: Hose barbs, cap nuts, seals
040296
Set. 4pcs, straight, GL14, silicone seal
Content: Hose barbs, cap nuts, seals
037642
Set. 6pcs, bent (4), straight (2), GL14, silicone seal
Content: Hose barbs, cap nuts, seals
038000
Further wear parts
Screw caps, set. 5pcs, GL14
040624
Cap nuts, set. 10pcs, screw cap with hole, GL14, incl. FEP seal
Content: Hose barbs, cap nuts, seals
041999
Operation Manual Rotavapor® R­100
55/60
10 | Appendix
BÜCHI Labortechnik AG
Cap nuts, set. 10pcs, cap nuts with hole, GL14
10.2.5
56/60
041956
Spare parts
Drain disc. PTFE, Ø5.1/14mm
040625
Top cover. For C condenser, PETP
027479
Seal, set. For C/CR condenser, PTFE, EPDM
027462
Screw couppling, set. Couppling, pressure spring
048237
Rubber band. To fasten condenser
032013
Cross sleeve. To fasten condenser
Not included: Rubber band (032013)
027344
Condenser C. Cold trap, 500m2
040645
Condenser V. Vertical condenser, 1460cm2
11055921
Cold finger. For C condenser
000672
Cold trap mantle. For C condenser
040641
Stopcock. For C condenser, glass
040628
Tubing. PTFE, Ø3/4mm, white, 600mm
Utilization: Feeding
028096
Screw cap. GL10
023875
Operation Manual Rotavapor® R­100
BÜCHI Labortechnik AG
10.3
10.4
Appendix | 10
List of abbreviations
Abbreviation
Meaning
ADR
Accord européen relatif au transport international des marchan­
dises dangereuses par route (European Agreement concerning the
International Carriage of Dangerous Goods by Road)
DKD
Deutscher Kalibrierdienst (German Calibration Service)
EPDM
Ethylene propylene diene monomer
FEP
Fluorinated ethylene propylene
FFKM
Perfluoro­elastomer
FPM
Fluorinated propylene monomer
GGVE
Gefahrgutverordnung Eisenbahn (German Hazardous Goods Reg­
ulations for Railways)
GGVS
Gefahrgutverordnung Strasse (German Hazardous Goods Regula­
tions for Road Transport)
NBR
Nitrile butadiene rubber
PBT
Polybutylene terephthalate
PETP
Polyethylene terephthalate
PTFE
Polytetrafluoroethylene
RID
Règlement concernant le transport international ferroviaire de
marchandises dangereuses (Regulations concerning the Interna­
tional Carriage of Dangerous Goods by Rail)
Health and safety approval
To guarantee the health and safety of our staff and to comply with the law and the reg­
ulations 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 Labortech­
nik AG or repaired unless we have received the declaration below, completed and
signed.
Products sent to us will not be accepted for repair or DKD calibration until we have re­
ceived this declaration.
u Copy the form overleaf and complete it.
u Make sure that you know the full details of the substances with which the device
has been in contact and the all questions have been answered fully and correctly.
u Send the completed from to us in advance by post or fax. The declaration must
reach us before the device.
u Enclose a copy of the declaration with the device.
u 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 mea­
sures.
Operation Manual Rotavapor® R­100
57/60
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 reg­
ulations 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 compo­
nents 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 We hereby assure that the products returned
non­hazardous
have not been used in the laboratory and are new.
materials
have not been in contact with toxic, corrosive, biologically active, explosive, ra­
dioactive or other hazardous materials.
are not contaminated. The solvents or residues of the substances pumped have
been removed.
Declaration for In respect of the products returned, we hereby assure that
hazardous materi­
all substances (toxic, corrosive, biologically active, explosive, radioactive or other­
als
wise 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 prod­
ucts 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:
58/60
Operation Manual Rotavapor® R­100
www.buchi.com
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