Operation Manual
Mini Spray Dryer B-290
093001 en
Table of contents
1 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6
2 Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7
2.1 User qualification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.2 Proper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.3 Improper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
2.4 Safety warnings and safety signs used in this manual . . . . . . . . . . . . . . . . . . 8
2.5 Product safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.5.1 General hazards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.5.2 Warning labels on housing and assemblies . . . . . . . . . . . . . . . . . . . . . . 14
2.5.3 Personal protective equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.5.4 Safety elements and measures . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.6 General safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
3 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3.1 Scope of application and delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3.1.1 Standard instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3.1.2 Standard accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
3.1.3 Standard accessories with the B-290 Advanced . . . . . . . . . . . . . . . . . . . 18
3.1.4 Standard accessories with the B-290 Acid resistant. . . . . . . . . . . . . . . . . . 18
3.1.5 Optional accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
3.2 Technical data overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
3.3 Materials used. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
4 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
4.1 Functional principle of the drying gas . . . . . . . . . . . . . . . . . . . . . . . . . 22
4.2 Functional principle of the sample feed and dispersion . . . . . . . . . . . . . . . . 22
4.3 Outlet filter. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
4.4 Inert Loop B-295 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
4.5 Dehumidifier B-296 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
4.6 Spray chilling accessory. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.7 Connected accessories to the Mini Spray Dryer B-290 . . . . . . . . . . . . . . . . 25
4.7.1 Feed switch valve and remote control panel. . . . . . . . . . . . . . . . . . . . . . 26
4.7.2 Printer or PC for data output via RS-232 serial port . . . . . . . . . . . . . . . . . . 26
5 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
5.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
5.2 Electrical connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
5.3 Installing the compressed air maintenance unit and compressor (optional) . . . . . . 28
5.4 Installing the glass assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
5.5 Installing the spraying nozzle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
5.6 Installing the filters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
5.6.1 Inlet filter installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
5.6.2 Outlet filter installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
5.6.3 PTFE filter membrane installation . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
5.6.4 Cleaning filter installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
5.7 Adjusting the peristaltic pump bed and choosing the feeding tube . . . . . . . . . . 35
5.8 Tubing installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
5.9 Installing the compressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
5.10 Quick hose couplings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
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3 B-290 Operation Manual, Version I
5.11 Installing the Inert Loop B-295 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
5.12 Dehumidifier B-296 and Inert Loop B-295 combination . . . . . . . . . . . . . . . . 42
5.13 Installing the Dehumidifier B-296 . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
5.14 Installing the Spray Chilling Accessory. . . . . . . . . . . . . . . . . . . . . . . . . 44
5.15 Installation check . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
5.16 Additional cleaning measures for food, pharma and cosmetic applications . . . . . . 46
5.16.1 Primary cleaning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
6 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
6.1 Layout of the operating and display elements . . . . . . . . . . . . . . . . . . . . . 48
6.2 Conversion tables for the parameters . . . . . . . . . . . . . . . . . . . . . . . . . 49
6.2.1 Flow meter spraying air (rotameter) . . . . . . . . . . . . . . . . . . . . . . . . . . 49
6.2.2 Peristaltic pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
6.2.3 Aspirator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
6.3 Spray process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
6.4 Optimizing parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
6.5 End of spray process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
6.6 Recovering particles of the outlet filter . . . . . . . . . . . . . . . . . . . . . . . . . 51
6.7 Operation with the Inert Loop B-295 . . . . . . . . . . . . . . . . . . . . . . . . . 53
6.7.1 Status messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
6.8 Operation with the Spray Chilling Accessory. . . . . . . . . . . . . . . . . . . . . . 55
6.9 Mini Spray Dryer B-290 acid resistant . . . . . . . . . . . . . . . . . . . . . . . . . 56
7 Maintenance and repairs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
7.1 Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
7.2 Glass assembly, tubes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
7.3 Nozzles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
7.4 Aspirator cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
7.5 Inert Loop B-295 and Dehumidifier B-296. . . . . . . . . . . . . . . . . . . . . . . 59
7.6 Outlet filter. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
7.7 Calibrating the oxygen sensor of the Inert Loop B-295 . . . . . . . . . . . . . . . . 60
7.8 Replacing the oxygen sensor of the Inert Loop B-295 . . . . . . . . . . . . . . . . . 61
7.9 Spray chilling accessory. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
7.10 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
8 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
8.1 Error messages and their remedy . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
8.2 Malfunctions and their remedy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
9 Shutdown, storage, transport and disposal . . . . . . . . . . . . . . . . . . . . . . . . 65
9.1 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
9.2 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
10 Spare parts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
10.1 Spray nozzle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
10.2 Glass parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
10.3 Filters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
10.4 Tubings and connectors. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
10.5 Trolley . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
10.6 Measurement pipe for gas flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
10.7 Feed switch valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
10.8 Remote control panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
10.9 Inert Loop B-295 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
10.10 Cylinder insulation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75
10.11 Spray chilling accessory. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76
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4 B-290 Operation Manual, Version I
10.12 Decontamination Glass-Set and sterile filter . . . . . . . . . . . . . . . . . . . . . . 77
10.13 Acid resistant accessories. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78
11 Declarations and requirements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79
11.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . . . . 79
11.2 Declaration of conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
11.3 Safety certificate. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81
11.4 Health and safety clearance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82
Table of contents
5 B-290 Operation Manual, Version I
1 About this manual
This manual describes the Mini Spray Dryer B-290 and its optional accessories and provides all information required for its safe operation and to maintain it in good working order.
It is addressed to laboratory personnel and operators in particular.
Read this manual carefully before installing and running your system and note the safety precautions
in chapter 2 in particular. Store the manual in the immediate vicinity of the instrument, so that it can be
consulted at any time.
No technical modifications may be made to the instrument without the prior written agreement of
BUCHI. Unauthorized modifications may affect the system safety or result in accidents. Technical data
are subject to change without notice.
NOTE
The symbols pertaining to safety are explained in chapter 2.
This manual is copyright. 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.
1 About this manual
The English manual is the original language version and serves as basis for all translations into other
languages. If you need another language version of this manual, you can download other versions at
www.buchi.com or reorder manuals from a BUCHI representative.
Abbreviations
EPDM: Ethylene Propylene Dimonomer
FFKM: Perfluoroelastomers
FPM: Fluoroelastomer
PEEK: Polyetheretherketone
PTFE: Polytetrafluoroethylene
POM: Polyoxymethylene
PFA: Perfluoroalkoxy
6 B-290 Operation Manual, Version I
2 Safety
This chapter highlights out the safety concept of the instrument and contains general rules of behavior
and warnings from direct and indirect hazards concerning the use of the product.
For the users safety, all safety instructions and safety messages in the individual sections shall
be strictly observed and followed. Therefore, the manual must always be available to all persons
performing any tasks described herein.
2.1 User qualification
The instrument is designed and built in accordance with state-of-the-art technology. Nevertheless, risks
to users, property, and the environment can arise when the instrument is used carelessly or improperly.
The manufacturer has determined residual dangers emanating from the instrument
• if the instrument is operated by insufficiently trained personnel without supervision.
• if the instrument is not operated according to its proper use.
Appropriate warnings in this manual serve to make the user alert to these residual hazards.
Personnel without this training or persons who are currently being trained require careful instruction.
The present Operation Manual serves as the basis for this.
2 Safety
2.2 Proper use
The Mini Spray Dryer B-290 has been designed and built as laboratory instrument and for batch
production. It serves to spray-dry aqueous solutions or suspensions in one operating process.
In combination with the Inert Loop B-295, it is possible to work with organic solvents in “closed
mode”. Processing in “closed mode” requires N2 or CO2 as an inert gas.
The output particle size of the Mini Spray Dryer B-290 is between 2–25 µm. Thus, the instrument is
suited to generate particles in the inhalable size range from a solution of suspension.
• If the instrument is used with potentially toxic or hazardous substances in ‘open mode’, it has
to be installed inside a closed fume hood or glove box. In such cases, the complete processing
and system handling has to be performed within the ventilated box to avoid toxication and other
hazardous situations to the user and the environment.
• Spray drying of corrosive samples require handling in a closed fume hood. An acid proof system in
open loop is a variant of the Mini Spray Dryer B-290.
• In any case, all exhausts leaving the exhaust gas tubing have to be lead away instantly by a ventilation system, to remove possibly hazardous substances and fumes from the working area. The
ventilation system has to be equipped with safety measures such as outlet filters to avoid contamination of the environmen.
• Operation and handling can require additional personal protective equipment. Operate the instrument with respect to standard laboratory safety rules (i.e. as stated in the latest version of the WHO
“Laboratory biosafety manual”) at all times.
• If the Mini Spray Dryer B-290 is used in combination with other instruments (e.g. Chiller) all related
manuals are to be fully observed.
• Electrostatic charges are to be arrested from both the product collection vessel and the cyclone via
the standard grounding cable if the cyclone is equipped with a grounding socket.
• If the instrument is used for food, pharma and cosmetic products additional cleaning measures
(primary cleaning and in place disinfection) are required (see chapter 5.7).
7 B-290 Operation Manual, Version I
2.3 Improper use
Applications not mentioned in section 2.2 are considered to be improper. Also, applications which do
not comply with the technical data (see section 3 of this manual) are considered to be improper. The
operator bears the sole risk for any damages or hazards caused by such improper use.
The following uses are expressly forbidden:
• Use of gases with unknown chemical composition.
• Spray drying of biohazardous materials such as viruses or bacteria.
• Spray drying of organic solvents without safety lamella curtain, Inert Loop B-295 and in open mode.
• Use of the instrument in rooms which require ex-protected instruments.
• Spray drying of substances which might explode or ignite due to the processing and the selected
parameters of the Mini Spray Dryer B-290 or installed sub systems.
• Spray drying of toxic substances.
• Use of samples which might produce oxygen during the processing.
• Unattended use.
2.4 Safety warnings and safety signs used in this manual
2 Safety
DANGER, WARNING, CAUTION and NOTICE are standardized signal words for identifying levels of
hazards and risks related to personal injury and property damage. All signal words, which are related
to personal injury are accompanied by the general safety sign.
For your safety it is important to read and fully understand the table below with the different signal
words and their definitions!
Sign Signal word Definition Risk level
DANGER
WARNING
CAUTION
NOTICE
no
Supplementary safety information symbols may be placed in a rectangular panel on the left to the
signal word and the supplementary text (see example below).
Space for
supplementary
safety
information
symbols.
!
Supplementary text, describing the kind and level of hazard/risk seriousness.
• List of measures to avoid the herein described, hazard or hazardous situation.
• ...
• ...
Indicates a hazardous situation which, if not avoided, will
result in death or serious injury.
Indicates a hazardous situation which, if not avoided, could
result in death or serious injury.
Indicates a hazardous situation which, if not avoided, may
result in minor or moderate injury.
Indicates possible property damage, but no practices
related to personal injury.
SIGNAL WORD
★★★★
★★★☆
★★☆☆
★☆☆☆
(property damage only)
8 B-290 Operation Manual, Version I
2 Safety
Table of supplementary safety information symbols
The reference list below incorporates all safety information symbols used in this manual and their
meaning.
Symbol Meaning
General warning
Electrical hazard
Heavy weight, avoid over exertion
Explosive gases, explosive environment
Harmful to life-forms
Hot item, hot surface
Device damage
Inhalation of substances
Chemical burns by corrosives
Fragile components
Wear laboratory coat
9 B-290 Operation Manual, Version I
2 Safety
Wear protective goggles
Wear protective mask
Wear protective gloves
Additional user information
Paragraphs starting with NOTE transport helpful information for working with the device/software or its
supplementaries. NOTEs are not related to any kind of hazard or damage (see following example).
NOTE
Useful tips for the easy operation of the instrument/software.
2.5 Product safety
Safety warnings in this manual (as described in section 2.4) serve to make the user alert and to avoid
hazardous situations emanating from residual dangers by giving appropriate counter measures.
However, risks to users, property and the environment can arise when the instrument is damaged,
used carelessly or improperly.
2.5.1 General hazards
The following safety messages show hazards of general kind which may occur when handling the
instrument. The user shall observe all listed counter measures in order to achieve and maintain the
lowest possible level of hazard.
Additional warning messages can be found whenever actions and situations described in this manual
are related to situational hazards.
!
DANGER
Death by suffocation or serious poisoning by inhalation of inert gases.
• Do not inhale inert gases
• Directly withdraw released gases and gaeous substances by sufficient ventilation
• Only operate the instrument in ventilated environments
• Before opertation, check all parts, connections and sealings involved in the gasflow for proper
sealing
• Exchange worn out or defective parts immediately
10 B-290 Operation Manual, Version I
2 Safety
!
DANGER
Death or serious poisoning by gases or particles due to O2- sensonr or filter malfunction
• Exchange defective O2-sensor immediately
• Exchange O2-sensor regularly within the specified maintenance intervals
• Exchange clogged filters immediately
• Exchange filters regularly within the specified maintenance intervals
• Dispose of filter immediately
!
DANGER
Death or serious poisoning by inhalation or incorporation of dried particles during spray process.
• Wear safety goggles
• Wear safety gloves
• Wear a suitable protective mask
• Wear a laboratory coat
• Check for proper sealing before use
• Do not inhale dried particles
• Stop drying gas flow before opening the drying circuit
11 B-290 Operation Manual, Version I
!
DANGER
Death or serious posioning by inhalation or incorporation of dried particles at recovery.
• Wear safety goggles
• Wear safety gloves
• Wear a suitable protective mask
• Wear a laboratory coat
• Do not inhale dried particles
• Stop drying gas flow before opening the drying circuit
• Only recover particles in sufficiently ventilated flue or glove-box
• Do not disperse the dried particles
• Do not clean dusty parts with compressed air
2 Safety
!
WARNING
Death or serious injuries by use in explosive environments.
• Do not operate the instrument in explosive environments
• Do not operate the instrument with explosive gas mixtures
• Before operation, check all gas connections for correct installation
• Directly withdraw released gases and gaseous substances by sufficient ventilation
12 B-290 Operation Manual, Version I
!
WARNING
Death or serious poisoning by contact or incorporation of harmful substances at use.
• Before operation, check the instrument for correct assembling
• Before operation, inspect sealings and tubes for good condition
• Exchange worn out or defective parts immediately
• Exchange clogged filters immediately
• Only operate the instrument in ventilated environments
• Directly withdraw released gases and gaseous substances by sufficient ventilation
• Perform a dry-run without sample material and check for gas leakages
!
CAUTION
Risk of minor poisoning by inhalation of ozone.
• Directly withdraw released gases and gaseous substances by sufficient ventilation
2 Safety
!
CAUTION
Risk of minor or moderate burnings when handling hot parts.
• Do not touch hot parts
• Let the system cool down for some minutes after use
!
NOTICE
Risk of instrument short-circuits and damage by liquids.
• Do not spill liquids over the instrument or its component parts
• Wipe off any liquids instantly
• Place the sample vessel onto the designated reservoir-plate on top of the instrument
• Ensure a safe positioning of the sample vessel
• Do not move the instrument when it is loaded with liquid
• Keep external vibrations away from the instrument
!
NOTICE
Risk of instrument damage by internal overpressure.
• External supply pressure must meet the system specifications
• Exchange clogged filters immediately
• Dispose of filter immediately
13 B-290 Operation Manual, Version I
!
NOTICE
Risk of instrument damage by wrong mains supply.
• External mains supply must meet the voltage given on the type plate
• Check for sufficient grounding
2.5.2 Warning labels on housing and assemblies
The following warning sticker(s) can be found on the housing or assemblies of the Mini Spray Dryer
B-290 and Inert Loop B-295:
Symbol Meaning Location
2 Safety
2.5.3 Personal protective equipment
Always wear personal protective equipment such as protective eye goggles, protective clothing and
gloves. Wear protective mask to protect from inhalation of fine particles. The personal protective
equipment must meet all requirements of all data sheets for the chemicals used. These instructions
are an important part of the instrument and must be made available at all times to the operating
personnel at the place where the equipment is deployed. Additional protective measures can
be necessary according to the applications! The user is fully responsible for choosing adequate
measures!
Do not touch
hot item, hot
surface!
See text Sticker at the rear side, B-290
See text Sticker/label, located on the B-295
Label, located at the spray cylinder,
B-290
14 B-290 Operation Manual, Version I
!
WARNING
Serious chemical burns by corrosives.
• Observe all data sheets of the used chemicals
• Handle corrosives in well ventilated environments only
• Always wear protective goggles
• Always wear protective gloves
• Always wear protective clothes
• Do not use damaged glassware
• Wear protective mask when working with inhalable particles
2.5.4 Safety elements and measures
2 Safety
To arrest electrostatic charges from the instrument, it is internally grounded. Electrostatic charges are
to be arrested from both the product collection vessel via the external (yellow) grounding cable for all
cyclones with grounding socket.
Heating
• Excess temperature protection against uncontrolled overheating.
• Automatic temperature control of the heater and inlet temperature.
• Heater can not be started before the closed loop is inert
Spraying (Pump)
• Pump can not be started before the closed loop is inert
Air/Gas
The system can be used in suction mode (standard) or in pressure mode. The suction procedure used
in the Mini Spray Dryer B-290 produces a light negative pressure in the instrument and thus rules out,
together with the inlet filter and outlet filter, a contamination of the environment through leaking from
the instrumen.
Automatic processing interruption when system pressure is too low in closed mode
• Outlet filter to protect the environment contamination of fine dust particles via exhaust gas tubing
N2 inert gas
The Mini Spray Dryer B-290 Advanced can be used to work with organic solvent in combination with
the Inert Loop B-295.
• Inertization against explosive gas mixtures
• oxygen concentration measurement (inside the Inert Loop B-295)
• pressure measurement (inside the Inert Loop B-295)
The heater and the pump stop if the oxygen level is > 6 vol.% or if the pressure level is < 10 mbar.
15 B-290 Operation Manual, Version I
Glass
• Use of inert 3.3 borosilicate glass.
• Grounded coating of the inner surface of the cyclone to prevent any electrostatic charge of the
power.
• Screw couplings between glass connections to prevent glass breakage.
Optional system configuration with Inert Loop B-295
• Overpressure leakage detection.
• Safe gas condition (< 6 % O2 content) is detected and enables the regulation of the drying gas
mixture via a communication cable.
2.6 General safety rules
Responsibility of the operator
The head of the laboratory is responsible for training his/her personne.
The operator shall inform the manufacturer without delay of any safety-related incidents which might
occur during operation of the instrument or its accessories. Legal regulations, such as local, state and
federal laws applying to the instrument or its accessories must be strictly followed.
2 Safety
Duty of maintenance and care
The operator is responsible for the proper condition of instrument. This includes maintenance, service
and repair jobs that are performed and on schedule by authorized personnel only.
Spare parts to be used
Use only genuine consumables and spare parts for maintenance to assure good system performance,
reliability and safety. Any modifications of spare parts or assemblies are only allowed with the prior
written permission of the manufacturer.
Modifications
Modifications to the instrument are only permitted after prior consultation and with the written approval
of the manufacturer. Modifications and upgrades shall only be carried out by an authorized BUCHI
technical engineer. The manufacturer will decline any claim resulting from unauthorized modifications.
16 B-290 Operation Manual, Version I
3 Technical data
This chapter introduces the reader to the instrument specifications. It contains the scope of delivery,
technical data, requirements and performance data.
3.1 Scope of application and delivery
The Mini Spray Dryer B-290 is available in three different set-ups:
Mini Spray Dryer B-290 Basic
• For aqueous applications with air in ‘open mode’
Mini Spray Dryer B-290 Acid resistant
• For acidic applications with air in ‘open mode’
Mini Spray Dryer B-290 Advanced
• For solvent applications in combination with Inert Loop B-295
• Optional use with Dehumidifier B-296
• Accessories are solvent resistant
3 Technical data
The scope of delivery can only be checked according to the individual delivery note and the listed
order numbers.
NOTE
For additional information on the listed products, see www.buchi.com or contact your local dealer.
3.1.1 Standard instrument
Table 3-1: Standard instrument
Product Order number
Mini Spray Dryer B-290 200 V 44781
Mini Spray Dryer B-290 230 V 44780
Mini Spray Dryer B-290 Advanced 200 V 44700
Mini Spray Dryer B-290 Advanced 230 V 44699
Mini Spray Dryer B-290
Acid resistant 200 V
Mini Spray Dryer B-290
Acid resistant 230 V
11056420
11056421
17 B-290 Operation Manual, Version I
3.1.2 Standard accessories
3 Technical data
Table 3-2: Standard accessories
Product Order number
Operation Manual:
German 093000
English 093001
French 093002
Italian 093003
Spanish 093004
Glass assembly complete 044680
Compressed gas tube, 5 m with quick
coupling, complete
046356
Silicone tube for nozzle cooling, 4 m 004139
Silicone tube (per m) 004138
Cleaning brush for nozzle 044782
Polypress tube for gas stream, 3 m 046341
Hose clamps 004236
Spray Dryer Application Support and
910040
Training (1 day training and application
tests)
3.1.3 Standard accessories with the B-290 Advanced
3.1.4 Standard accessories with the B-290 Acid resistant
Table 3-3: Standard accessories with the B-290
Advanced
Product Order number
Lamella safety curtain 044783
Feed switch valve 044725
Spray cylinder, vertical outlet 044697
Nozzle cap, 1.4 mm 044649
Tygon tube MH 2075 transparent (per m) 046314
Tygon tube F 4040 A yellow (per m) 046315
Table 3-4: Standard accessories with the B-290
Acid resistant
Product Order number
Two-fluid nozzle acid resistant 11056320
Glass assembly acid resistant complete 11056386
Spray cylinder holder PFA coated 11056324
Cyclone metall cover PFA coated 11056327
Knurled screws PFA coated 11056325
Flange coupling PFA coated 11056326
Temperature sensor acid resistant 11056329
18 B-290 Operation Manual, Version I
3.1.5 Optional accessories
3 Technical data
Table 3-4: Standard accessories with the B-290
Acid resistant (cont.)
Temperature sensor support adapter 11056318
Clamp ring ID 8 mm 11056387
O-ring FPM 8×1 mm 004221
Connecting nipple PFA coated 11056328
Connecting piece PFA coated 11056334
Needle 0.7 mm titanium 11056415
Nozzle tip 0.7 mm titanium 11056317
Table 3-5: Optional accessories
Product Order number
Inert Loop B-295 50 Hz, 200 V 044779
Inert Loop B-295 50 Hz, 230 V 044701
Inert Loop B-295 60 Hz, 200 V 046345
Inert Loop B-295 60 Hz, 230 V 046344
Dehumidifier B-296 50/60 Hz, 230 V 040188
Dehumidifier B-296 50/60 Hz, 200 V 040181
Spray chilling accessory 50/60 Hz, 230 V 040351
Spray chilling accessory 50/60 Hz, 200 V 040352
Brown glass assembly 044758
Two-fluid nozzle, complete 044698
Three-fluid nozzle, complete 046555
Three-fluid nozzle conversion kit 046556
Three-fluid nozzle acid resistant 11056971
Cylinder Insulation 040058
Remote control panel B-290 044702
Outlet filter acid resistant complete 11056333
Outlet filter, complete 044754
Inlet filter 011235
Compressed air maintenance unit 004366
Oil-free compressor, 230 V/50 Hz 027907
Oil-free compressor, 230 V/60 Hz 11055737
IQ/OQ Documentation B-290 11057023
OQ Documentation B-290 11057024
19 B-290 Operation Manual, Version I
3.2 Technical data overview
Table 3-6: Technical data Mini Spray Dryer B-290
Power consumption max. 2900 W
Connection voltage 200–230 V ± 10 %
Frequency 50/60 Hz
Environmental conditions
Temperature
Altitude
Humidity
Evaporating capacity 1.0 l/h H2O, higher for organic solvents
Airflow max. of 35 m3/h
Motor control Frequency converter
Max. temperature input 220 °C
Heating capacity 2300 W
Heating control PT-100, fuzzy logic, control accuracy ± 2 °C
Interface Serial port RS-232 for all parameters
Spray gas Compressed air or nitrogen/200–800 l/h, 5–8 bar
Nozzle tip diameter 0.7 mm standard, other sizes 1.4 and 2.0 mm available
Possible particle diameter range 1–25 µm
Mean residence time 1.0–1.5 sec.
Pollution degree 2
Installation category II
Dimensions (W×H×D) 65×110×70 cm
Weight 46 kg
3 Technical data
for indoor use only
5–40 °C
up to 2000 m
maximum relative humidity 80 % for temperatures up to
31 °C decreasing linearly to 50 % relative humidity at 40 °C
Table 3-7: Technical data Spray Chilling accessory
Power consumption max. 400 W
Connection voltage 200–230 V ± 10 %
Frequency 50/60 Hz
Heating control (from B-290) PT-100, fuzzy logic, control accuracy ± 2 °C
Interface Serial port RS-232 for all parameters
Spray gas Compressed air or nitrogen/200–800 l/h, 5–8 bar
Nozzle tip diameter 0.7 mm standard, other sizes 1.4 and 2.0 mm available
Possible particle diameter range 20–200 µm
Mean residence time 1.0–1.5 sec.
Pollution degree 2
Installation category II
Dimensions (W×H×D) 20×20×30 cm
Weight 2.4 kg
Product vessel 87 mm height, 71 mm inner ∅
Batch volume 0.3 liter
20 B-290 Operation Manual, Version I
3 Technical data
Table 3-7: Technical data Spray Chilling accessory (cont.)
Heating liquid water or a thermal oil (polyethylene glycol PEG 400 with
low viscosity)
Heating liquid volume 1.4 liter
Max. melting point of sample 70 °C
Table 3-8: Technical data Inert Loop B-295
Power consumption max. 1400 W
Connection voltage 200-230 V ± 10 %
Frequency 50/60 Hz
Min. outlet temperature down to –25 °C
Rate of cooling 800 W at –10 °C
Dimensions (W×H×D) 60×70×84.5 cm
Weight 88 kg
Table 3-9: Technical data Dehumidifier B-296
Power consumption 700 W
Connection voltage 200/230 V ± 10 %
Frequency 50/60 Hz
Min. outlet temperature + 2 °C
Rate of cooling 600 W at 0 °C
Dimensions (W×H×D) 35×40×60 cm
Weight 36 kg
3.3 Materials used
Table 3-10: Materials used
Component Material designation Material code
Glass assembly 3.3 borosilicate glass
Nozzle/heater/connection piece Stainless steel 1.4301/1.4305
Seal of product collection vessel FPM (FFKM)
Seal cyclone/cylinder Silicone
Preheat exchanger Inert Loop B-295 Stainless steel 1.4301
Polypress tube EPDM
Product feed tube Silicone and tygon
Molecular sieve bag of adsorption unit PEEK
Acid resistant coated metal PFA (perfluoroalkoxy polymer)
Acid resistant metal titanium, Alloy 600
Metal parts Mini Spray Dryer B-290 acid
resistant
PFA-coated
21 B-290 Operation Manual, Version I
4 Description of function
This chapter explains the basic working principle of the Mini Spray Dryer B-290 Basic (open mode
only) and the Mini Spray Dryer B-290 Advanced (for closed mode operation). It also shows how the
instruments are structured and provides a general functional description of the assemblies.
4.1 Functional principle of the drying gas
The Mini Spray Dryer B-290 operates according to a co-current drying gas (e.g. air in open mode)
and product stream. This means that sprayed product and hot gas have the same flow direction from
downward.
2
1
3
4
5
7
4 Description of function
a Gas inlet (optional with attached inlet filter)
b Electric heater
8
c Concentric inlet of the hot gas around the
spray nozzle
d Spray cylinder
e Cyclone to separate particles from gas
stream
f Product collection vessel
g Outlet filter
h Aspirator to pump gas through system
6
Fig. 4.1: Functional principle of the drying air
4.2 Functional principle of the sample feed and dispersion
The Mini Spray Dryer has a integrated two-fluid nozzle: Compressed gas (normally air or N2) is used to
disperse the liquid body into fine droplets which are subsequently dried in the cylinder.
a Feed solution
4
5
Fig. 4.2: Functional principle of the sample feed and dispersion
6
3
2
1
b Peristaltic pump
c Two fluid nozzle
d Connection for cooling water
e Connection for compressed spray gas
f Automatic nozzle cleaning system
Spraying nozzle
The nozzle consists of the nozzle tip with a 0.7 mm dia meter hole and the nozzle cap
(1.4 or 1.5 mm in diameter). This geometry results in a mixing of fluid body and gas.
22 B-290 Operation Manual, Version I
The nozzle cap has an inserted ruby stone with a precise opening and sharp edges to guaran tee a
N
precise and reproducible spray cone.
The smaller nozzle cap of 1.4 mm diameter leads to a lower consumption of spray gas, as the
concentric ring around the nozzle is smaller. This nozzle is recommended when nitrogen is used to
minimize operating costs. The larger nozzle cap opening of 1.5 mm is typically used when air serves
as spraying gas, as this design is more robust regarding concentric alignment to form a vertical and
uniform spray cone.
Optional nozzle sets with 1.4 mm or 2.0 mm nozzle tip diameter are available to increase the droplet
size and/or to spray more viscous samples or dispersions.
4.3 Outlet filter
The outlet filter, consisting of a polyester textile, prevents environmental pollution and the possible
corrosion of the aspirator by very fine particles which cannot be separated in the cyclone. It can be
washed by hand or machine. All needed connections are included.
The second filter included is made of a PTFE membrane. By counter-pulsing the filter with pressurised
air, some of the collected particles can be reco vered resulting in a higher yield (see chapter 6.6.
The manometer indicates the system pressure in front of the filter. With a clean filter, the corresponding
pressure drop is marked.
4 Description of function
4.4 Inert Loop B-295
Mini Spray Dryer B-290
Advanced
2
1
a Feed
b Product
c Exhaust gas
d Solvent
Fig. 4.3: Combined system of the Mini Spray Dryer B-290 and Inert Loop B-295
Inert Loop B-295
5
6
7
2
3
4
e Preheat exchanger
f Condensation
g Cooling unit
The Inert Loop B-295 is an accessory to enable the safe use of organic solvent in a closed loo.
The inert gas is loaded with solvent from the spray drying process. After precooling in a preheat
exchanger, the solvent is condensed in a refrigerator and collected in a closed bottle. The cleaned
gas stream is preheated in the preheat exchanger and flows back to the Mini Spray Dryer B-290
Advanced.
23 B-290 Operation Manual, Version I
4.5 Dehumidifier B-296
4 Description of function
Dehumidifier B-296
Mini Spray Dryer B-290
8
7
1
2
3
4
a Ambient air
b Condensation
c Cooling unit
d Condensed water
Fig. 4.4: Open loop Mini Spray Dryer B-290 with Dehumidifier B-296 for inlet air conditioning
5
e Product
f Exhaust gas
g Compressed air as spray gas
h Feed
6
Use as inlet air conditioning
The Dehumidifier B-296 is an accessory to enable a drying under constant and reproducible humidity
conditions cooling to a dew point of 3–5 °C.
The drying air is passing the refrigerator of the Dehumidifier B-296. The humidity in the ambient air
condenses in the refrigerator and is collected in a closed bottle.
The dry air is then heated up by the heater of the Mini Spray Dryer B-29.
Use in the closed mode
The Dehumidifier B-296 is an accessory to enable the safe use of a water-organic solvent mixture in a
closed loop with up to 50 % organic solvents content.
The inert gas is loaded with water-solvent mixture from the spray drying process in an external preheat
exchanger.
The solvent condenses in the Dehumidifier B-296 and is collected in a receiving vessel.
24 B-290 Operation Manual, Version I
4.6 Spray chilling accessory
During spray chilling a hot melt is dispersed into a cold gas stream. The droplets are solidified into
particles and are separated. The matrix substance and the active ingredients are heated above the
melting point. Highest melting point is 70 °C. The nozzle is also heated to prevent any blocking. No
additional thermostat is required, as the existing heating control and peristaltic pump in the instrument
are used. If the sample has a low melting point, then the inlet air is cooled to increase the temperature
gradient. If lower temperatures than 10 °C (provided by the B-296) are used, e.g. for hard fats, the
inlet air can be cooled to –5 °C by using a specially developed refrigeration unit (please contact your
local distributor.
1
4
4 Description of function
a Temperature sensor
b Circulating heating liquid to bath – nozzle –
peristaltic pump – bath
c Cold gas
d Heated feed sample
e Droplets spray
2
3
5
Fig. 4.5: Functional principle of the sample feed and dispersion
4.7 Connected accessories to the Mini Spray Dryer B-290
a Serial port RS-232 for data output to a PC
b Connection for the remote control panel
c Connection for Inert Loop B-295
1
Fig. 4.6: Rear connections of the Mini Spray Dryer B-290
2
3 4
d Connection for feed switch valve
25 B-290 Operation Manual, Version I
4.7.1 Feed switch valve and remote control panel
Fig. 4.7: Feed switch valve and remote control panel
The remote control panel enables an easy operation even within a closed fume hood. The flow meter
for the spraying gas is the only parameter which cannot be adjusted via the remote control panel.
The feed switch valve is a useful tool together with the remote control panel. During the start and end
of the spray process, the feeding tube has to be moved from pure solvent to product solution and
vice versa. This can be automated by means of the feed switch valve. A Y-piece is inserted between
peristaltic pump and feed switch valve.
4 Description of function
4.7.2 Printer or PC for data output via RS-232 serial port
The Mini Spray Dryer B-290 is supplied with a standard protocol for data readout. This is of special
importance if the system is qualified and underlies special regulations.
The connection starts as soon as the heater is switched on.
The transmission rate is 2400 Baud/s, Parity: No.
The parameters are sent out every 30 seconds as an ASCII-Code, separated by a TAB (ASCII 09)
and ended with a RETURN (ASCII 0D). They can be read out e.g. via the program “HyperTerminal”
included in the Microsoft package.
The source is defined as follows:
No. Information Type Unit
1 Time since mains on integer s
2 Current temperature inlet integer °C
3 Current temperature outlet integer °C
4 Heater on/off 0/1
5 Set temperature inlet integer °C
6 Aspirator on/off 0/1
7 Aspirator rotation speed integer %
8 Pump on/off 0/1
9 Pump rotation speed integer %
10 Feed switch valve 1/2
11 Connection Inert Loop B-295 no/yes 0/1
12 Oxygen high 0/1
13 Pressure low 0/1
14 Error message integer
26 B-290 Operation Manual, Version I
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