BUCHI B-90 User Manual

Operation Manual
Nano
Spray Dryer B�90
093261
en
Table of contents
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 signals used in this manual . . . . . . . . . . . . . . . . . 8
2.5 Product safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.5.1 General hazards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.5.2 Warning labels on housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.5.3 Safety measures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.5.4 Built-in safety elements and measures . . . . . . . . . . . . . . . . . . . . . . . . 14
2.6 General safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
3 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
3.1 Scope of application and delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
3.1.1 Standard instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
3.1.2 Standard accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3.1.3 Standard accessories with the Nano Spray Dryer B-90 Advanced. . . . . . . . . . . 19
3.1.4 Optional accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
3.2 Technical data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
3.3 Materials used. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
4 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.1 Functional principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.1.1 Drying gas circuit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
4.1.2 Spray drying process overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
4.2 Spray generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
4.3 Heating system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
4.4 Drying air generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
4.4.1 Compressed air supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
4.4.2 Aspirator in blowing mode. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
4.5 Sample feed circulation with peristaltic pump . . . . . . . . . . . . . . . . . . . . . 29
4.6 Particle collector. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
4.7 Outlet filter. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
4.8 Inert Loop B-295 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
4.9 Dehumidifier B-296 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
4.10 Connection at the Nano Spray Dryer B-90 . . . . . . . . . . . . . . . . . . . . . . 33
If you need another language version of this manual, you can download available versions at www.buchi.com.
3 B-90 Operation Manual, Version B
Table of contents
5 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
5.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
5.2 Installing the Nano Spray Dryer B-90 . . . . . . . . . . . . . . . . . . . . . . . . . 35
5.2.1 Tall set-up with long metal bars . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
5.2.2 Short set-up with short metal bars . . . . . . . . . . . . . . . . . . . . . . . . . . 36
5.3 Sub-assembly installations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
5.3.1 Lifting device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
5.3.2 Electrode assembly installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
5.3.3 Glass cylinder installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
5.3.4 Heater module installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
5.4 Spray head assembling and installation . . . . . . . . . . . . . . . . . . . . . . . . 43
5.4.1 Spray head assembling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
5.4.2 Spray head installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
5.5 Peristaltic pump and feed tubing installation. . . . . . . . . . . . . . . . . . . . . . 47
5.5.1 Peristaltic pump height adjustment and fixation . . . . . . . . . . . . . . . . . . . . 48
5.5.2 Pump bed adjustment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
5.5.3 Feeding tube installation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
5.6 Drying gas supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
5.6.1 ‘open loop’ air supply configuration . . . . . . . . . . . . . . . . . . . . . . . . . . 52
5.6.2 ‘closed loop’ gas supply configuration. . . . . . . . . . . . . . . . . . . . . . . . . 53
5.6.3 Outlet filter installation/replacement . . . . . . . . . . . . . . . . . . . . . . . . . . 53
5.7 Aspirator installation modes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
5.7.1 Aspirator in ‘open loop’ configuration . . . . . . . . . . . . . . . . . . . . . . . . . 54
5.7.2 Aspirator in ‘closed loop’ configuration . . . . . . . . . . . . . . . . . . . . . . . . 55
5.8 Inert Loop B-295 installation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.8.1 Main device installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
5.9 Dehumidifier B-296 installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
5.9.1 Dehumidifier B-296 in ‘open loop’ configuration . . . . . . . . . . . . . . . . . . . . 59
5.9.2 Dehumidifier B-296 in ‘closed loop’ configuration with out Inert Loop B-295 . . . . . 60
5.9.3 Adsorption column installation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
5.10 Final installation check. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
5.11 Electrical connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
6 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
6.1 Starting up the instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
6.2 Main screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
6.3 Menu structure overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
6.4 Display elements and menu functions . . . . . . . . . . . . . . . . . . . . . . . . . 65
6.4.1 Operating controls. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
6.4.2 View parameters menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
6.4.3 Gas mode selection menu. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
6.4.4 Configuration menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
6.4.5 Firmware calibration menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
6.4.6 Firmware info menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
6.5 Starting a spray drying process . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
6.6 Optimizing parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71
6.7 End of spray drying process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
6.8 Collecting the particles from the collector cylinder . . . . . . . . . . . . . . . . . . . 72
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Table of contents
6.9 Other operation modes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
6.9.1 Inert Loop B-295 operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
6.9.2 Dehumidifier B-296 operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75
6.10 Using the Nano Spray Dryer Records software on a PC. . . . . . . . . . . . . . . . 76
7 Maintenance and repairs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83
7.1 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84
7.2 Housing condition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84
7.3 Glass component conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84
7.4 Oxygen sensor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
7.5 Sealing conditions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
7.6 Cleaning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
7.6.1 Spray head and tube connections. . . . . . . . . . . . . . . . . . . . . . . . . . . 85
7.6.2 Outlet filter. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
7.6.3 Inert Loop B-295 and Dehumidifier B-296. . . . . . . . . . . . . . . . . . . . . . . 86
8 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87
8.1 Error messages and their remedy . . . . . . . . . . . . . . . . . . . . . . . . . . . 87
8.2 Malfunctions and their remedy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
9 Shutdown, storage, transport and disposal . . . . . . . . . . . . . . . . . . . . . . . . 91
9.1 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91
9.2 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
10 Spare parts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
10.1 Spray head . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
10.2 Glass parts and mounting items. . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
10.3 Particle collector, heater and lifting device items . . . . . . . . . . . . . . . . . . . . 96
10.4 Filters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
10.5 Tubing and accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
10.6 Inert Loop B-295, Dehumidifier B-296 and Adsorption Column . . . . . . . . . . . . 98
11 Declarations and requirements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .100
11.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . . . .100
11.2 Declaration of conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .101
5 B-90 Operation Manual, Version B
1 About this manual
This manual describes the Nano Spray Dryer B-90 and provides all information required for its safe operation and to maintain it in good working order. It is addressed to laboratory personnel in particular.
Abbreviations
EPDM Ethylene Propylene Dimonomer FFKM Perfluoroelastomers FPM Fluoroelastomer PEEK Polyetheretherketone PTFE Polytetrafluoroethylene (Teflon)
PE Polyethylene PVC Polyvinylchloride
1 About this manual
6 B-90 Operation Manual, Version B
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 chapters shall be strictly observed and followed. Therefore, the manual must always be available to all persons performing the tasks described herein.
2.1 User qualification
The instrument may only be used by laboratory personnel and other persons who on account of training and professional experience know of the potential dangers that can develop when operating the instrument.
Untrained personnel, or persons who are currently being trained, require careful supervision by a quali­fied person. The present Operation Manual serves as a basis for training.
2 Safety
2.2 Proper use
The Nano Spray Dryer B-90 and the Nano Spray Dryer B-90 Advanced have been designed and built as laboratory instruments.
The Nano Spray Dryer B-90 serves to spray-dry aqueous solutions or suspensions in ‘open loop’ with compressed air as drying gas.
The Nano Spray Dryer B-90 Advanced can additionally process organic solvent solutions or suspensions in ‘closed loop’ when combined with the Inert Loop B-295. Processing in ‘closed loop’ requires N2 or CO2 as an inert gas.
The output particle size of the Nano Spray Dryer B-90 is between 300 nm–5 µm. Thus, the instru­ment is ideally suited to encapsulate particles and nano particles (<100 nm) from a solution or suspension.
If the instrument is used with potentially toxic or hazardous substances in ‘open loop’, 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.
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 environment. When the Nano Spray Dryer B-90 is used in combination with other instruments (e.g.
Aspirator) all related manuals are to be fully observed.
7 B-90 Operation Manual, Version B
2.3 Improper use
Applications not mentioned in section 2.2 are considered to be improper. Applications which do not comply with the technical data (see section 3 of this manual) are also considered to be improper.
The operator bears the sole risk for any damages or hazards caused by improper use!
The following uses are expressly forbidden:
• Use of gases with unknown chemical composition.
• Spray drying of biohazard materials such as viruses or bacteria.
• Spray drying of organic solvents in ‘open loop’ and without the Inert Loop B-295.
• Installation or 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 Nano Spray Dryer B-90 or installed sub systems.
• Use of samples which might produce oxygen during the processing.
2 Safety
2.4 Safety warnings and safety signals used in this manual
DANGER, WARNING, CAUTION and NOTICE are standardized signal words for identifying levels of hazard seriousness of 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 below table with the different signal words and their definitions!
Sign Signal word Definition Risk level
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.
no
DANGER
WARNING
CAUTION
NOTICE
★★★★
★★★☆
★★☆☆
★☆☆☆
(property damage only)
Supplementary safety information symbols may be placed in a rectangular panel on the left to the signal word and the supplementary text (see below example).
!
SIGNAL WORD
Space for
supplementary
safety
information
symbols.
8 B-90 Operation Manual, Version B
Supplementary text, describing the kind and level of hazard / risk seriousness.
List of measures to avoid the herein described, hazard or hazardous situation.
...
...
2 Safety
Table of supplementary safety information symbols The below reference list incorporates all safety information symbols used in this manual and their
meaning.
Symbol Meaning
General warning
Electrical hazard
Explosive gases, explosive environment
Harmful to life-forms
Hot item, hot surface
Device damage
Inhalation of substances
Pressurized gas/air
Ozone formation
Wear protective mask
9 B-90 Operation Manual, Version B
Wear laboratory coat
Wear protective goggles
Wear protective gloves
Heavy weight, lifting requires more than one person
2 Safety
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 example below).
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.
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2 Safety
!
Danger
Death by suffocation or serious poisoning by inhalation of inert gases.
Do not inhale inert gases
Directly withdraw released gases and gaseous substances by sufficient ventilation
Only operate the instrument in ventilated environments
Before operation, check all parts, connections and sealings involved in the gasflow for proper sealing
Exchange worn out or defective parts immediately
!
Danger
Death or serious poisoning by gases or particles due to O2– sensor 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-90 Operation Manual, Version B
!
Danger
Death or serious poisoning 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
!
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
12 B-90 Operation Manual, Version B
!
Caution
Risk of minor poisoning by inhalation of ozone.
Directly withdraw released gases and gaseous substances by sufficient ventilation
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
2 Safety
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
Risk of instrument damage by internal overpressure.
External supply pressure must meet the system specifications
Exchange clogged filters immediately
Dispose of filter immediately
Risk of instrument damage by wrong mains supply.
External mains supply must meet the voltage given on the type plate
Check for sufficient grounding
Notice
Notice
Notice
13 B-90 Operation Manual, Version B
2.5.2 Warning labels on housing
The below warning label can be found at the gas outlet connector on the right side of the Nano Spray Dryer B-90.
Meaning Ozone formation in the electric field of the electrostatic particle collector when using oxygen containing
gases as drying gas (like air). Withdraw gases via fume hood or equivalent ventilation system directly.
2 Safety
2.5.3 Safety measures
Always wear personal protective equipment such as protective eye goggles, protective clothing, inha­lation protection and gloves when working with the instrument.
2.5.4 Built-in safety elements and measures
Heating
• Overheating protection circuit.
• Automatic temperature control of heater and inlet temperature.
Spraying
• Automatic spray control.
• Light barrier, to detect the correct placement of the particle collector.
• Overpressure leakage detection.
High voltage and electrostatic charges
• Safety current limitation.
• Internal grounding to arrest electrostatic charges.
Air/Gas
• Automatic processing interruption when system pressure is too low.
• Outlet filter to protect the environment contamination of fine dust particles via exhaust gas tubing.
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Glass
• High temperature resistance and high transparency borosilicate glass.
Pressure
• Automatic pressure control at outlet filter.
• Over pressure safety valve (opens at 300 mbar).
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 personnel.
The operator shall inform the manufacturer without delay of any safety-related incidents which might occur during operation of the instrument. Legal regulations, such as local, state and federal laws applying to the instrument must be strictly followed.
2 Safety
Duty of maintenance and care The operator is responsible for the proper condition of instrument at use and that maintenance,
service and repair jobs are performed with care and on schedule by authorized personnel only.
Spare parts to be used Use only genuine consumables and genuine spare parts for maintenance to assure good system
performance and reliability. Any modifications to the spare parts used are only allowed with the prior written permission of the manufacturer.
Modifications Modifications to the instrument are only permitted after prior consultation with 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.
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3 Technical data
This chapter introduces the reader to the instrument and its specifications. It contains the scope of delivery, technical data, requirements and performance data.
3.1 Scope of application and delivery
The Nano Spray Dryer B-90 is available in two different set-ups:
Nano Spray Dryer B-90 Basic
For aqueous applications with air in ‘open loop’
Nano Spray Dryer B-90 Advanced
For solvent applications in combination with Inert Loop B-295
Optional use with Dehumidifier B-296
Equipped with additional oxygen safety circuit and gas regulation valves
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 about the listed products, see www.buchi.com or contact your local dealer.
3.1.1 Standard instrument
Table 3-1: Standard instrument
Product Order no.
Nano Spray Dryer B-90 Basic 50 – 60 Hz, 100 – 240 V
Nano Spray Dryer B-90 Advanced 50 – 60 Hz, 100 – 240 V
11055320
11055321
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3.1.2 Standard accessories
3
3 Technical data
Table 3-2: Standard accessories
Product Order no.
Spray head 051510
Spray head holder 051508
Set of 3 spray caps 4.0 µm 051747
Set of 3 spray caps 5.5 µm 051748
Set of 3 spray caps 7.0 µm 051749
HV–Electrode protected 11055174
Protective grid for HV–Electrode 051680
Peristaltic pump complete 051735
17 B-90 Operation Manual, Version B
3 Technical data
Table 3-2: Standard accessories (cont.)
Product Order no.
Spray cylinder 051511Glass cylinder extension 051549
Glass insulation cylinder (no picture) 051663
1
Heater complete 051504
Lifting device 051607
«Nano Spray Dryer Records» Software 051776
18 B-90 Operation Manual, Version B
Operation Manual
Nano
Spray Dryer B�90
3 Technical data
Table 3-2: Standard accessories (cont.)
Product Order no.
Outlet filter 051656
Operation Manual:
English 093261
German 093262
French 093263
Italian 093264
Spanish 093265
093261
Deckblatt B-90_en.indd 1 08.07.2009 09:44:56
en
3.1.3 Standard accessories with the Nano Spray Dryer B-90 Advanced
Table 3-3: Standard accessories with the B-90
Product Order no.
Oxygen sensor 046348
Tygon tubing MH 2075 transparent (per m) 046314
Tygon tubing F 4040 A yellow (per m) 046315
Upgrade set Nano Spray Dryer B-90 Basic to Advanced
NOTE
Upgrade set is for organic solvent operation in ‘closed loop’ with the Inert Loop B-295 or Dehu­midifier B-296. The upgrade set includes solvent resistant tubing, inert gas regulation valves, oxygen sensor with oxygen analyser. The installation requires support of a BUCHI service engi­nee r.
Advanced (for ‘closed loop’ operation)
11055748
19 B-90 Operation Manual, Version B
3.1.4 Optional accessories
3 Technical data
Table 3-4: Optional accessories
Product Order no.
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
Upgrade set B–295 for closed cycle 051783
Dehumidifier B-296, 50/60 Hz, 230 V 040188
Dehumidifier B–296, 50/60 Hz, 200 V 040181
Upgrade set B–296 for closed cycle 051780
Aspirator complete, incl. inlet filter 051700
20 B-90 Operation Manual, Version B
3 Technical data
Table 3-4: Optional accessories (cont.)
Product Order no.
Inlet filter 011235
Air maintenance unit 004366
Oil-free air compressor, 230V / 50Hz 027907
Oil-free air compressor, 230V / 60Hz 11055736
Trolley 041257
21 B-90 Operation Manual, Version B
3.2 Technical data
Table 3-5: Technical data Nano Spray Dryer B-90
Power consumption max. 1500 W Connection voltage 100–240 VAC ± 10 %
Input fuse 12 A
Frequency 50 / 60 Hz
Heating capacity max. 1400 W
Max. inlet temperature 120 °C
Evaporating capacity max. 0.2 l/h H2O
Drying gas flow 80–160 l/min
N2 or CO2 inert gas input pressure max. 2 bar
Spray caps (hole diameters) 4.0 µm, 5.5 µm, 7.0 µm
Mean droplet size range 8–21 µm
Mean particle size range 300 nm–5 µm
Mean residence time 1–4 sec.
Interface USB II
IP degree of protection (two digits) IP 42
3 Technical data
Table 3-4: Optional accessories (cont.)
Product Order no.
Stand plate 051775
(higher rates with organic solvents are possible)
Explanation of protection level:
4 Protection provided by the enclosure against access
to hazardous parts (e.g., electrical conductors, moving parts) and the ingress of solid foreign objects with a diameter of > 1mm.
2 Protection of the equipment inside the enclosure
against harmful ingress of dripping water when tilted up to 15°.
Overvoltage category II
Environmental conditions:
Pollution degree 2 (for indoor use only)
Temperature 5–40 °C
Altitude (above sea level) up to 2000 m
Humidity (curve parameter) Maximum relative humidity 80 % up to 31 °C, then
decreasing linearly to 50 % relative humidity at 40 °C
22 B-90 Operation Manual, Version B
Table 3-5: Technical data Nano Spray Dryer B-90 (cont.)
Dimensions (W × H × D)
Short set-up 58×110×55 cm Tall set-up 58×150×55 cm
Weight
Short set-up 65 kg
Tall set-up 70 kg
Table 3-6: Technical data Inert Loop B-295
Power consumption max. 1.4 kW
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 95 kg
3 Technical data
Table 3-7: 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
Table 3-8: Technical data Aspirator
Power consumption max. 1000 W
Connection voltage 200–240 V ± 10 %
Input fuse FST 5×20 T8A L 250 V
Frequency 50/60 Hz
Dimensions (W×H×D) 47,5×30×32 cm
Weight 20 kg
IP degree of protection (two digits) IP 20
Explanation of protection level:
2 Protection provided by the enclosure against access
to hazardous parts (e.g., electrical conductors, moving parts) and the ingress of solid objects up to 12 mm, e.g. persons fingers.
0 No protection against ingress of liquids.
23 B-90 Operation Manual, Version B
3.3 Materials used
Table 3-9: Materials used
Component Material designation
Glass assembly 3.3 borosilicate glass
Heater Aluminum and stainless steel
Spray head Stainless steel
Spray cap membrane Stainless steel
Spray cap o-ring EPDM75
Feeding tubes Silicone and tygon
Tube connector at feeding tube PEEK
Particle collecting tube Stainless steel polished
HV–electrode Stainless steel
Sealings for spray and glass cylinder Silicone
3 Technical data
24 B-90 Operation Manual, Version B
4 Description of function
This chapter explains the basic working principle of the Nano Spray Dryer B-90 Basic (‘open loop’ only) and the Nano Spray Dryer B-90 Advanced (equipped with O2-sensor and inert gas regula­tion valves for ‘closed loop’ mode). It also shows how the instruments are structured and provides a general functional description of their assemblies.
4.1 Functional principle
The Nano Spray Dryer B-90 models have been designed to produce particles out of a solution or suspension with a particle size between 0,3 µm–5 µm by drying or encapsulation at a yield rate of up to 90 %. The output particle size depends mainly upon the chosen spray cap. The Nano Spray Dryer B-90 also allows processing of nano particles (<100 nm) in nanosuspensions or emulsions e.g. for encapsulation. The drying gas flow and the product stream are described below.
4.1.1 Drying gas circuit
4 Description of function
The sprayed liquid is accompanied by a co-current gas flow. For highest yields, a controlled gas flow at a sufficient quality and a defined temperature is required. To ensure this, a flow regulator and heating loop has been implemented
a The drying and transport gas enters the instrument
a
Drying gas inlet
via the “Drying gas inlet”.
b The gas flow is monitored by a “Flow meter”
which influences the “Gas regulator”.
Gas regulator
b
Flow meter
Feed pump
c Subsequently the “Electrical heater” heats up the
gas to the desired drying temperature.
c
Electrical heater
Spray head
d Via the “Inlet temperatur sensor” the heater is
regulated to achieve the desired gas temperature.
d
Inlet temp. sensor
e The “Relative pressure sensor” compares the in-
ternal to the environmental pressure. In the event of a massive pressure loss (e.g. a leakage) this
f
safety loop
Drying cylinder
sensor stops the drying process.
f In ‘closed loop’ mode, as part of the safety loop
Electrical particle
collector
the “Oxygen sensor” supervises the percentage of oxygen in the drying gas. In emergency, it stops the process.
Oxygen sensor
e
Rel. pressure sensor
g The “Outlet temperature sensor” is located after
the particle collector. The temperature drop
g
Outlet temp. sensor
h
Outlet filter
i
Drying gas outlet
between inlet and outlet temperature sensor is measured as a process value.
h The “Outlet filter” is a safety relevant item. It re-
tains possibly harmful particles towards the envi­ronment in ‘open loop’. In ‘closed loop’ the outlet filter is an essential part for cleaning the recycled gas from unwanted residues and impurities.
i The “Drying gas outlet” works as an exhaust.
25 B-90 Operation Manual, Version B
Optional drying gas recycling in ‘closed loop’ mode: In ‘closed loop’ mode of the Nano Spray Dryer B-90 Advanced the “Drying gas outlet” i is connected
via the Inert Loop B-295 or Dehumidifier B-296 and Aspirator to the “Drying gas inlet” a.
4.1.2 Spray drying process overview
The drying process takes place inside the drying cylinder. A drying gas flow is established and tiny droplets of sample material are injected by the spray head. The sample material is dried by the hot gas. Because of the tiny particle size, an electrical field of sufficient power is needed to retrieve the particulate material from the drying gas flow. The following scheme informs about the different processing stages in general.
Drying gas inlet
Gas regulator
safety loop
Flow meter
Electrical heater
Inlet temp. sensor
Drying cylinder
Electrical particle
c
d
collector
a
Feed pump
b
Spray head
4 Description of function
a The “Feed pump” constantly feeds the “Spray head”
with liquid sample material.
b The “Spray head” produces finest droplets and in-
jects them into the “Drying cylinder”.
c The heated drying gas enters laminar from the top
into the “Drying cylinder”. Consequently, the injected drops of sample material are gently dried to solid particles.
d The “Electrical particle collector” retrieves the dried
solid particles by an electrostatic field.
e The exhaust gas leaves the spray dryer via the “Out-
let filter” which retains free particles from the gas.
Oxygen sensor
Rel. pressure sensor
Outlet temp. sensor
e
Outlet filter
Drying gas outlet
26 B-90 Operation Manual, Version B
4 Description of function
pull pull
Processing inside the drying cylinder The following draft offers a more detailed view about the basic spray drying process. The drying
gas (a) passes the heater (b) and the vertically or angular aligned spray head (e). The injected micro doplets of the sample material are dried while beeing vortexed in the gas flow inside the spray cylinder (f). An electric field is generated by high voltage between the collecting electrode (h) and the HV-electrode (i). While the HV-electrode deflects the particulate material, the collecting electrode attracts them. Thus, particles are depositing at the inside of the collecting electrode (g).
a


c



f


h
i

4.2 Spray generation
The Nano Spray Dryer B-90 uses piezotechnology to generate precisely controlled micro droplets from bulk liquids without the use of propellants.

b
e


j



k
g
d
l
a Drying gas inlet (optional with inlet filter and Aspira-
tor)
b Electrical heater c Inlet temperature sensor d Display/Control e Spray head (angular or vertical installation) f Spray cylinder and drying section g Finished product at particle collecting electrode h Particle collecting electrode i HV–electrode j Outlet temperature sensor k Outlet filter l Drying gas outlet (in ‘closed loop’ connected to Inert
Loop B-295 and Aspirator)
push
NOTE
The smaller the mesh size, the smaller the ejected droplets and dried particles. Since the vibrations frequency is fixed, a smaller mesh size will have less throughput per time.
4.3 Heating system
The compact heater module provides optimal energy input to heat the drying gas up to 120 °C. The heating system consists of an electrically heated porous metal foam to minimize the heat–up time and to generate a laminar gas flow towards the drying section. The heating control is based on a plug­gable PT–1000 temperature sensor.
push
The spray head includes a piezoelectric actuator with a thin stainless steel membrane. The membrane has an array of micron-sized holes (spray meshes of 4.0,
5.5 or 7.0 µm hole size) and vibrates at ultrasonic frequency (60 kHz). Because of these vibrations the membrane eject precisely sized droplets at high speed.
27 B-90 Operation Manual, Version B
4.4 Drying air generation
In ‘open loop’ mode the required drying air can be either supplied by an in-house compressed air supply, an oil-free compressor or a BUCHI Aspirator (see section 3.1.4, Optional accessories).
4.4.1 Compressed air supply
In ‘open loop’ configuration, compressed air is used as standard drying gas. The air maintenance unit (order no. 004366) is additionally recommended to assure gas of clean, dry and oil free quality. A pres­sure regulating valve is required to match the instruments input pressure value.
Nano Spray Dryer B-90
Basic
4 Description of function
Air maintenance unit
T
IN
P
Product
T
OUT
a Compressed air source b Optional air maintenance unit c Pressure regulating valve
4.4.2 Aspirator in blowing mode
If there is no compressed air available in the laboratory, the BUCHI Aspirator unit with inlet filter (order no. 051700) can be used to establish the required drying air flow rate. The Aspirator can be connected directly to the inlet of the Nano Spray Dryer B-90 without a pressure regulating valve. In case of higher ambient humidity use the Dehumidifier B-296 to achieve dry air.
Feed
Control
FI
Outlet filter
c
Exhaust gas
Compressed
air
b (optional)
a
NOTE
If the humidity of the air is too high, the current in the particle collector could be too low.
Air inlet filter The air inlet filter is required to avoid any contamination of the instruments by fine particles in the lab
environment. It is to be connected to the inlet of the Aspirator, so the instrument aspirates filtered ambient air. The filter consists of a stainless steel grid for outer protection and an ultra filter based on a glass fibre textile (filter class S according to DIN 24184).
28 B-90 Operation Manual, Version B
Nano Spray Dryer B-90
Basic
Feed
T
IN
Control
Dehumidifier
B-296
T
COOL
4 Description of function
c (optional)
Aspirator
P
Product
T
OUT
a Inlet filter to filter out dust and particles b Aspirator as air supply source c Optional Dehumidifier B-296
FI
Condensate
Exhaust gas
Outlet filter
NOTE
The Aspirator is also used with a Nano Spray Dryer B-90 Advanced in ‘closed loop’ configuration with the Inert Loop B-295 or Dehumidifier B-296 to recirculate the inert gas (N2 or CO2).
4.5 Sample feed circulation with peristaltic pump
The peristaltic pump circulates the sample feed between the product vessel and the spray head. It assures a constant substance feeding for the spray generation.
b
a
Inlet filter
NOTE
Dry run of the pump and the spray head does not damage the instrument or parts of it in the medium term.
4.6 Particle collector
Solid particles are accumulated at the wall of the cylindrical particle collecting electrode by a strong electrical field. The electrical field is generated via high voltage.
4.7 Outlet filter
The outlet filter (order no. 051656) prevents environmental pollution by particles. It is installed inside the housing of the Nano Spray Dryer B-90. See section 5.5.1 for information about access and exchange.
29 B-90 Operation Manual, Version B
4.8 Inert Loop B-295
The Inert Loop B-295 is an accessory to enable the safe spray drying of organic solvents in a ‘closed loop’ configuration. It comprises a cooling unit with pressure and oxygen monitoring elements and safety controls. Communication to the Nano Spray Dryer B-90 Advanced is established via a commu­nication cable.
Product
4 Description of function
a
Exhaust gas
T
COOL
Dehumidifier
a Exhaust gas to fume hood or glove box ventilation
outlet
b Solvent condensate
B-296
c Condensation and cooling unit
c
b
Functional principle:
• The inert drying gas (N2 or CO2) is loaded with solvent from the spray drying process.
• The loaded gas enters the Inert Loop B-295 and is cooled down in its internal preheat exchanger.
• The solvent is condensed in the refrigerator and collected in a closed bottle.
• Subsequently, the cleaned and cooled gas stream is heated up in the preheat exchanger and flows back through an Aspirator to the Nano Spray Dryer B-90 Advanced.
Dehumidifier B-296 If mixtures of organic solvents and water are used in ‘closed loop’ configuration, BUCHI strongly
recommends to install the additional Dehumidifier B-296. The Dehumidifier B-296 is condensing the water to prevent water from entering the Inert Loop B-295. This is necessary to protect the heat
exchanger in the refrigerator from water freezing and potential damage.
30 B-90 Operation Manual, Version B
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