b290 (1)
b290 (1)
Operation Manual
093001M en
093001M en
BÜCHI Labortechnik AG
Meierseggstrasse 40
Postfach
CH-9230 Flawil 1
E-Mail: [email protected]
BUCHI reserves the right to make changes to the manual as deemed necessary in the light of experience; espe-
cially in respect to structure, illustrations and technical detail.
This manual is copyright. Information from it may not be reproduced, distributed, or used for competitive purpos-
es, nor made available to third parties. The manufacture of any component with the aid of this manual without
prior written agreement is also prohibited.
Table of contents
This manual describes the Mini Spray Dryer B-290 and its optional accessories and provides all infor-
mation 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 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.
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
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.
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.
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 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 ventila-
tion 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 contami-
nation of the environmen.
• Operation and handling can require additional personal protective equipment. Operate the instru-
ment 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 are
required.
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.
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!
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).
Symbol Meaning
General warning
Electrical hazard
Harmful to life-forms
Device damage
Inhalation of substances
Fragile components
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.
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
! 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
! 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
! 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
! 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
! 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
! 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
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:
Do not touch
Label, located at the spray cylinder,
hot item, hot
B-290
surface!
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!
! 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
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.
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.
3 Technical data
This chapter introduces the reader to the instrument specifications. It contains the scope of delivery,
technical data, requirements and performance 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.
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)
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.
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.
a Gas inlet (optional with attached inlet filter)
b Electric heater
2
3 c Concentric inlet of the hot gas around the
8
1 spray nozzle
d Spray cylinder
4 e Cyclone to separate particles from gas
stream
f Product collection vessel
7 g Outlet filter
5
h Aspirator to pump gas through system
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 b Peristaltic pump
5 6
2 c Two fluid nozzle
d Connection for cooling water
e Connection for compressed spray gas
3 f Automatic nozzle cleaning system
Spraying nozzle
The nozzle consists of the nozzle tip with a 0.7 mm diameter hole and the nozzle cap
(1.4 or 1.5 mm in diameter). This geometry results in a mixing of fluid body and gas.
The nozzle cap has an inserted ruby stone with a precise opening and sharp edges to guarantee a
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.
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 recovered 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.
6
7
2 3 4
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.
8
7
1
3 6
4 5
a Ambient air e Product
b Condensation f Exhaust gas
c Cooling unit g Compressed air as spray gas
d Condensed water h Feed
Fig. 4.4: Open loop Mini Spray Dryer B-290 with Dehumidifier B-296 for inlet air conditioning
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.
a Temperature sensor
1
b Circulating heating liquid to bath – nozzle –
peristaltic pump – bath
4 c Cold gas
d Heated feed sample
e Droplets spray
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:
This chapter describes how the instrument is installed and gives instructions on initial startup.
NOTE
Inspect the instrument for damages during unpacking. If necessary, prepare a status report immedi-
ately to inform the postal company, railway company or transportation company.
Keep the original packaging for future transportation.
Put the instrument on a stable, horizontal surface. Consider the maximum product dimensions and
weight and the operation height of 1.30 meters for spray chilling applications. Make sure that you can
comfortably reach the instrument.
Installation on a mobile trolley is also possible. Obtain the environmental conditions as described in
section 3.2, technical data.
! 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 without inertization
• Before operation, check all gas connections for correct installation
• Directly withdraw released gases and gaseous substances by sufficient ventilation
! Caution
Risk of minor or moderate injury by heavy weight of the instrument.
• Consult a second person to transport the instrument
• Do not tilt or drop the instrument
• Place the instrument on a stable, even and vibration-free surface
• Keep limbs out of crushing zone
• Lift the device at the right and left bottom reaching areas for the hands
The Mini Spray Dryer B-290 is aimed to be installed mobile and is and is shipped with a flexible power
cord. After the installation, an electrical safety test is recommended to verify a safe system condition
such as sufficient grounding.
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
NOTE
To cut the power in case of an emergency by unplugging, the instruments or any other items
must not block the mains plug! External connections and extension lines must be provided with a
grounded conductor lead (3-pole couplings, cord or plug equipment). All used power cords must
meet the input power requirements.
1 2
1 Heater connection
2 Power supply connection
5.3 Installing the compressed air maintenance unit and compressor (optional)
To ensure the Mini Spray Dryer B-290 achieves an optimal atomization performance, the supply of
compressed air with a pressure of 5–8 bar is necessary. The compressed air must be dried and free of
impurities (contamination of the product through impure air). If this is not guaranteed, we recommend
the use of a WILKERSON maintenance unit.
Notice
Risk of instrument damage by internal overpressure.
• External supply pressure must meet the system specifications
• Exchange clogged or defective filters immediately
• Dispose of clogged or defective filter immediately
1 2 3
If there is no compressed air plant available, the compressed air can be taken from an oil-free air
compressor with an output of 5– 8 bar as require.
! CAUTION
Risk of minor or moderate cuts by sharp edges.
• Do not touch defective or broken glassware with bare hands
• Do not touch thin metal edges
• A
ttach the cyclone k together with the
product collection vessel n to the connection
9 piece f with a second flange screw joint j.
• Screw the glass elbow i onto the top of the
cyclone.
• Connect the grounding cable l to the cover
10 of the product collection vessel m and to the
housing to minimize the electrostatic charge
11 of the powder.
6 4
12
13
14
15
Notice
Risk of instrument damage by internal overpressure.
• External supply pressure must meet the system specifications
• Exchange clogged or defective filters immediately
• Dispose of clogged or defective filters immediately
Use
Pre-filtering of environmental air to keep most impurities and particles away from the spray drying
process.
• U
nscrew all screw caps of the tubing at the filter head a and unhook the complete filter from the
holder.
• Unscrew the screw cap b and pull off the filter housing glass. Remove the sealing ring.
a
b
c
➡ Wash the polyester filter manually or in a laboratory washing machine. Use standard soap deter-
gents for cleaning.
For installation proceed in reverse order. Mind the correct mounting direction of the sealing ring (order
no. 040471) at the filter housing glass!
NOTE
The flange screw coupling made of aluminum (order no. 048539) is recommended for the use of
outlet temperatures higher than 80 °C for better sealing performance compared to the polymer
(POM) flange (order no. 034139).
c
a
filter tube
➡ Gently flush the PTFE filter membrane manually only. Use standard soap detergents for cleaning.
NOTE
Make sure the end-cap properly seals the filter carrier and the filter membrane! This is essential for
effective filtering.
Mind the correct mounting direction of the sealing ring (order no. 040471) at the filter housing glass!
NOTE
The flange screw coupling made of aluminum (order no. 048539) is recommended for the use of
outlet temperatures higher than 80 °C for better sealing performance compared to the polymer
(POM) flange (order no. 034139).
Use
• W hen connected to the air inlet at the heater the filter works as an inlet cleaning filter to remove
even finest particles from the drying air.
• When connected to the process air outlet tube the filter works as a safety element to hold back
finest product residues from the environmental air.
5.7 Adjusting the peristaltic pump bed and choosing the feeding tube
The pump bed of the peristaltic pump is adjusted ex works to the standard silicone tube.
If different tubes, e.g. the tygon tubes for organic solvents, are used, adjust the pump bed with an
allen key. Connect an adapter piece as a tube stopper between two feeding tubes to prevent slipping
in the peristaltic pump.
Adjusting the peristaltic pump bed
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
Choose the feeding tube according to the following table. For short processes, even unsuitable tubes
can be used, as swelling takes some time.
The Mini Spray Dryer B-290 needs compressed gas for the two-fluid nozzle and the nozzle cleaner
between 5 and 8 bar. Therefore, the air or nitrogen is connected on the rear of the instrument via a
quick coupling.
The Mini Spray Dryer B-290 can be used in an open or closed mode. The open mode is set in the
suction mode as a standard. However, if the exhaust gas is aggressive and could lead to a corrosion
of the aspirator, the instrument can also be run in a pressure mode. This mode leads to a higher noise
emission.
NOTE
Risk of instrument malfunction when the instrument is operated with bent hoses.
• Always inspect the instrument for bends or kinks in hoses and eliminate them prior to operation.
• Exchange hoses with signs of mechanical stress such as small cracks and blind spots at the
surface immediately.
2
1
Use
For the spray process compressed air or gas is necessary. If no compressed air supply is available in
the laboratory the compressor can be installed instead.
Installation
• Place it in a dry, dust free and well tempered room with appropriate ventilation.
• Follow the compressors manual to install the device.
• Connect the outlet of the compressor to the compressed air inlet of the Mini Spry Dryer B-290.
NOTE
Set the compressor to 6 bar output pressure to achieve recommended standard spray conditions.
Use
For fast and reliable connecting/disconnecting of polypress tubes e.g. the tubing of Inert Loop B-295
and Dehumidifier B-296.
Installation
• C
ut the polypress tube with a sharp knife or a special tube cutter into two halfs with a clean cut.
The tube ends must be straight!
• Slip one hose clamp over each tube end.
• Use one male and one female coupling adapter and install them at the tube ends.
• Secure the coupling adapters with the hose clamps.
• Test all tubes and connectors for tightness prior use!
Male coupling
! 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 clogged or defective filters immediately
! 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 ventilatio.
• Perform a dry-run without sample material and check for gas leakages
Fig. 5.19: Mini Spray Dryer B-290 Advanced with Inert Loop B-295 as trolley
1
3 5
Fig. 5.20: Tubing installation for closed mode operation with Mini Spray Dryer B-290 Advanced and Inert Loop B-295
NOTE
Disconnect the display from the front side and insert a LR 44 battery in the display.
Fig. 5.23: Tubing between the Mini Spray Dryer B-290 and the Dehumidifier B-296
Fig. 5.24: Tubing between the preheat exchanger and the Mini Spray Dryer B-290
Installation steps:
1. Place the Dehumidifier B-296 next to the Mini Spray Dryer B-290.
2. Connect the tubing b from the outlet (labelled on the enclosure) of the Dehumidifier B-296 to the
gas inlet of the Mini Spray Dryer B-290.
3. Connect the tubing a from the Mini Spray Dryer B-290 outlet to the inlet of the Dehumidifier
B-296 (labelled on the enclosure).
4. Use hose clamps to fix all Polypress tubings.
5. Connect the power cord to the mains. The device can now be switched on.
NOTE
See section 7.6 for information about the cleaning procedure of the Dehumidifier B-296.
NOTE
The nozzle tip 1.4 mm with nozzle cap 2.0 mm are recommended to increase the droplet size and if
clogging occurs with the standard 0.7 mm nozzle. The resulting particle size is typically in the order
of the droplet size.
Open suction mode installation with the Dehumidifier B-296 to pre-cool the inlet air is recommended.
A slight negative pressure in the spray chamber forces the melted sample feed to enter the nozzle
after opening the feed valve.
1
3
4
4 7
7 5
8 4
2 5
4
10
9
4 4
11
1
1 5
3
5
2
4 4
4
4
Carry out an installation check after a successful installation and prior to the first spray drying
process.
• Inspect the glass visually for possible damage.
• Check the electrical connections.
• Make sure that the cover of the product collection vessel is connected to the instrument by means
of the cable for arresting electrostatic charges.
• Make sure that the outlet temperature probe is inserted in the coupling.
6 Operation
This chapter gives examples of typical instrument applications and instructions on how to operate the
instrument properly and safely.
! 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
! 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
a Main switch
b Flow meter for spraying gas volume
c Needle valve for gas flow adjustment
1
3 4 5
6
1 2
14 12 10 8
7
15 13 11 9
a LED display current value inlet air temperature h Nozzle cleaner interval adjustment
b LED display current value outlet air temperature i Manual operation pneumatic nozzle cleaner
c LED display set value inlet air temperature j Regulating push-button pump
d LED display aspirator output in % of max. aspirator rate k Main switch pump
e LED display pump output in % of max. pump rate l Regulating push-button aspirator
f LED display for nozzle cleaning m Main switch aspirator
g Feed switch valve button n Regulating push-button heating
o Main switch heating
Fig. 6.2: Operating and display elements
The rotameter is an indicator for the spray gas flow. The table gives a correlation between indicated
height and volume throughput. The nozzle has a certain pressure drop which increases with higher
gas flow. As the gas volume strongly corresponds to the actual pressure, the table also contains a row
for the effective volume flow, determined in a spray process with air.
Height (mm) Liters/hour Pressure drop (bar) Actual volume flow (at standard
temperature and pressure)
in liters/hour
5 84
10 138
15 192
20 246 0.15 283
25 301 0.18 355
30 357 0.23 439
35 414 0.3 538
40 473 0.41 667
45 536 0.55 831
50 601 0.75 1052
55 670 1.05 1374
60 742 1.35 1744
65 819 1.8 2293
6.2.3 Aspirator
During the spray process some parts i.e. all glassparts can get hot according to the
temperature settings of the instrument!
! 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
The parameters relevant for the spray process (aspirator and pump performance as well as inlet
temperature) all correlate with and depend on each other. To give you an overview over the parameter
settings best suited for your process, special training papers can be downloaded directly from the
Internet.
Please visit our homepage www.buchi.com. In the section Fields of Activities/Spray Drying, you will
find the document to download.
• A fter the solution is completely spray dried, continue to spray pure solvent for a short time to
remove product deposits from the hoses and the nozzle. Air and solvent should alternate to ensure
an efficient cleaning.
• Pump the hoses empty, turn off the peristaltic pump and lower the pump bed.
• Turn off the nozzle cleaner.
• Turn off the heating. The system cools down now.
• As soon as the temperature in the instrument falls below 90 °C, you can turn off the aspirator.
• You can now remove the product collection vessel with the product.
• ATTENTION
Do not remove the product collection vessel when the aspirator is still on as the air stream might
blow the product out of the vessel into the surrounding area.
! 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
If the system is run with a PTFE filter, the fine particles can partially be recovered by counter-pulsating
the filter membrane and blowing the particles away. For this purpose, proceed as follows:
• A ttach the PTFE membrane instead of the polyester filter and close the bottom with a polypro-
pylene plug.
• Separate the manometer tube from the filter and remove the filter housing completely from the
holder.
• Put the filter on the product feed table. Disconnect the nozzle cleaning tube from the nozzle and
connect it to the filter housing.
• Close the outlet gas connection with an SVL 42 screw cap.
• With the nozzle cleaning set on level 1, a pressure blow is generated every 5 seconds on the inner
side of the filter leading to a separation of the fines from the membrane. The particles fall into the
glass and can be recovered.
! 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 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
a Switch on
b Switch off
c Temperature up
Temperature down
Display
Signal lamp oxygen
Signal lamp pressure
Signal lamp operation
Signal lamp power
Usually the Inert Loop is set on -20°C for optimal solvent recovery. Some solvents tend to freeze
in the Inert Loop B-295, while working with those please adjust the set temperature to a higher
one, use the buttons c and d. The display of the Inert Loop B-295 e shows the set tempera-
ture and the current temperature.
2. Switch on the aspirator (see figure 6.2 on page 52).
3. Check whether the spray gas source is an inert gas, normally nitrogen. Open the needle valve
at the flow meter and adjust the flow to the requested level. The closed system now starts to be
inertised (see figure 6.2 on page 52).
4. As soon as a certain pressure drop threshold is reached by the gas flow and spraying gas, the
signal lamp of the pressure display g is switched off. If the pressure drops under the threshold
(due to glass breakage, stop of gas inlet, taking away of a glass component etc.), the peristaltic
pump and the heater are blocked. This is indicated by a lit signal lamp g and the message PR
LO on the display of the Mini Spray Dryer B-290.
5. The overpressure in the system due to the constant flow inlet is limited by the exhaust outlet at
the Inert Loop B-295, which is permanently open. Therefore, no overpressure can built up. The
gas mixture from the exhaust outlet is slightly contaminated with solvents. This gas flow must
undergo an after treatment and be disposed of according to regional standards and laws.
6. The oxygen concentration decreases due to the constant inlet of inert gas. As soon as the
concentration is below 6 %, the signal lamp of the oxygen control f goes off. If the oxygen
threshold of 6 % is exceeded (e.g. by using pressurized air instead of inert gas), the peristaltic
pump and the heater are blocked. This is indicated by a lit signal lamp f and the message O2
HI on the display of the Mini Spray Dryer B-290.
7. As soon as both signal lamps f and g go off, the peristaltic pump and the heater are
unblocked and can be turned on. The spray process can be started. The blocking and signals
are reversible. If the pressure increases or the oxygen decreases, respectively, the pump and
heater are unblocked again and must be started manually.
8. At the left bottom side of the Inert Loop B-295 a flask is positioned to receive the condensed
solvent. To empty the flask, close the drain valve and take out the flask carefully.
NOTE
Do not use hydrochloric acid (HCl) for cleaning stainless steel.
Do not spray hydrochloric acid (HCl) because it will corrode the stainless steel parts.
This chapter gives instructions on all maintenance work to be performed in order to keep the
instrument in good working condition.
! Danger
Death or serious poisoning by inhalation or incorporation of dried particles during maintenance.
• Wear safety goggles
• Wear safety gloves
• Wear a suitable protective mask
• Wear a laboratory coat
• Clean all parts thoroughly
• Only maintain the instrument in ventilated environments
• Do not inhale dried particles
• Stop drying gas flow before opening the drying circuit
! Warning
Death or serious burning by electric current.
• Switch off the instrument, disconnect the power cord and prevent unintentional restart before
removing housing or parts of it
• Do not touch parts inside the instrument with wet hands
• Do not spill liquids over electronic components
• Do not squeeze cables, tubes or other items at reassembling
• Exchange defective cabling or tubing before reassembling
! Warning
Death or serious injuries by compressed air and gases.
• Depressurize air and gas circuit first
• Wear safety goggles
! CAUTION
Minor or moderate injuries by hot heating bath content.
• Do not drop any water into the hot heating liquid
• Wear safety goggles
Notice
Risk of instrument and instrument damage by liquids and detergents.
• Do not spill liquids over the instrument or parts of it
• Wipe off any liquids instantly
• Use ethanol or soapy water as detergent only
7.1 Housing
Check the housing for defects (switches, plugs) and clean it regularly with a damp cloth.
Clean the glass assemblies after each spray process. The glass assemblies can be taken out and
cleaned with commercially available cleaning agents or in an ultrasonic bath. After the glass parts
have been cleaned and fully dried, check each part visually for cracks, scratches and for any parts
or sections that might have splintered off. Take out and replace any damaged glass parts. Clean the
tubes after each spray process with commercially available cleaning agent.
7.3 Nozzles
A special brush is supplied to clean the central tube of the nozzle body. Most efficient cleaning of all
nozzle types is done in an ultrasonic bath. Clean the tubes and nozzles after each spray process.
The tubes and nozzles can be cleaned with commercially available cleaning agents.
The aspirator of the Mini Spray Dryers can be contaminated from particles, especially when no outlet
filter is used. This is a description how to clean the aspirator efficiently and fast.
Disconnect the “Polypress” tube from the
glass assembly and heater respectively.
• Fill one vessel with water and prepare an empty canister with a small opening.
• Insert the exhaust tube from the aspirator into one third of the empty canister and fix the tube.
• Set the aspirator to 50 % and switch it on. Carefully move the inlet tube over the surface of the
water to suck in a mixture of air and water.
• Do not immerse the tube into the water. Be aware that no splashes are contaminating the ambient
at the outlet side.
• Increase the aspirator rate up to 80 %, continue to draw water through the aspirator. Be careful,
that the exhaust tube in the receiving tank remains in the air to prevent splashes.
• Continue this procedure unless clean water is coming out of the aspirator.
• Let the aspirator run for approximately 1 hour to dry residual water in the aspirator away.
The sealed working circuits of the devices and the optional heat exchanger in combination with the
Inert Loop B-295 and Dehumidifier B-296 can be flooded completely for cleaning purpose.
Notice
Risk of instrument and instrument damage by liquids and detergents.
• Do not spill liquids over the instrument or parts of it
• Wipe off any liquids instantly
• Use ethanol or soapy water as detergent only
• Switch off all relevant devices and unplug the respective power cords.
• Remove the molecular sieve bag for the duration of cleaning if installed.
• Check all sealings and tubes for good condition and proper sealing.
• Raise the exhaust tube and fill the system through the inlet with cleaning medium (e.g. ethanol).
• Provide a collection vessel to collect the cleaning medium flowing from the system. Open the drain
valve and lower the exhaust tube, so that the cleaning medium flows out.
• Rinse out and dry the condensate vessel.
• Reinstall the condensate vessel.
• To dry the working circuit connect the Mini Spray Dryer B-290 and dry it by running the Aspirator
with dry air.
If the pressure drop of the outlet filter increases by more than 20 mbar relative to the clean filter, take
the filter out and wash it manually or in a laboratory washing machine or replace it by a new filter.
Notice
Risk of instrument damage by internal overpressure.
• External supply pressure must meet the system specifications
• Exchange clogged filters immediately
• Safely dispose filter immediately
The oxygen sensor is already calibrated ex works. However, due to shipping and other influences, the
sensor might have to be calibrated again. At atmospheric condition, it has to display 21.0 ± 1.5 %.
• Remove the small front plate with a screwdriver
1 2 3 4 • Remove the small front panel on the upper right side
with a screwdriver.
• Press menu d, C:01 will appear.
• Press UP b/DOWN a to change to C:02.
• Press Enter c, the oxygen concentration is shown on
the display.
• Press Enter c again to calibrate the sensor.
Fig. 7.2: Calibrating the oxygen sensor • Press Menu d to quit the menu mode.
After approximately 2 years of operation the oxygen concentration displayed by the sensor decreases
drastically.
The sensor should now be replaced. For this purpose:
• Open the front plate with an allen key.
• Disconnect the cable by turning the plug.
• Screw the sensor out and replace it by a new one.
• Reconnect the cable.
• Calibrate the sensor according to chapter 7.6, Cali-
brating the oxygen sensor.
Prior to cleaning, let the spray chilling accessory cool down with its covers on.
For cleaning, proceed as follows:
• Fill the spray chilling accessory with the cleaning agent and open the needle valve.
• If the accessory is blocked remove it.
• Use hot water, soap solutions and a brush for cleaning.
• Put the blocked metal parts in a heating oven to melt the stocked product.
• Wash all parts with water and let them dry.
• The silicone tubing between the spray chilling accessory and the nozzle has to be replaced if it is
blocked or broken.
Only authorised service personnel are allowed to perform repair work on the instrument. These
persons have a comprehensive technical training and knowledge of possible dangers which might
arise from the instrument.
Addresses of official BUCHI customer service offices are given on the BUCHI website under:
www.buchi.com. If malfunctions occur on your instrument or you have technical questions or applica-
tion problems, contact one of these offices.
The customer service offers the following:
• Spare part delivery
• Repairs
• Technical advice
8 Troubleshooting
This chapter helps to resume operation after a minor problem has occurred with the instrument. It lists
possible occurrences, their probable cause and suggests how to remedy the problem.
The troubleshooting table below lists possible malfunctions and errors of the instrument. The operator
is enabled to correct some of those problems or errors by him/herself. For this, appropriate corrective
measures are listed in the column “Corrective measure”.
The elimination of more complicated malfunctions or errors is usually performed by a BUCHI technical
engineer who has access to the official service manuals. In this case, please refer to your local BUCHI
customer service agent.
This chapter instructs how to shut down the instrument, how to pack it for storage or transport, and
specifies the storage and shipping conditions.
! WARNING
Death or serious poisoning by contact or incorporation of harmful substances.
• Wear safety goggles
• Wear safety gloves
• Wear a laboratory coat
• Clean the instrument and all accessories thoroughly to remove possibly dangerous substances
• Do not clean dusty parts with compressed air
• Store the instrument and its accessories at a dry place in its original packaging
Switch off the instrument and remove the power cord. Clean the instrument thoroughly! Remove all
liquids and dusty residues before packaging the instrument.
NOTE
When returning the instrument to the manufacturer for repair work, please copy and complete the
health and safety clearance form (section 11) and enclose it with the instrument.
9.2 Disposal
You have to follow valid regional and local laws concerning disposal.
NOTE
For help, please contact your local authorities!
10 Spare parts
This section lists spare parts, accessories and options including their ordering information.
Only order spare parts and consumables from BUCHI to maintain the warranty status and to assure
best performance and reliability of the system and affected components. Any modifications to the
spare parts used are only allowed with the prior written permission of the manufacturer.
Always state the product designation, instrument serial and part numbers for warranty clearance when
ordering spare parts!
044634
044618
044647
044649
046556
046377
046554
046375
Table 10-6: Standard O-rings FKM, for all standard to medium-aggressive applications
Description Order number
21.0×2.0 mm
16.0×2.0 mm
6.0×1.5 mm
004222
O-ring for nozzle cleaner, 038348
002103 FKM (black), 2×
3.0×1.5 mm
Table 10-7: Highly resistant O-rings FFKM, for all medium to aggressive applications
Description Order number
37.69×3.5 mm
6.0×1.5 mm
3.0×1.5 mm
046361
Set of FFKM O-rings, 046364
(002103) complete
Set, complete
046363
NOTE
O-rings in brackets are part of the standard O-ring set, order no. 044759!
004192
Seal to product collection vessel 040471
034139 Silicone seal SVL 42 040674
040471
044678 Angle piece 046333
Cylinder, sideways outlet 044673
Product collection vessel 044678
003551 004188 044678 Holder to spray cylinder 044710
040674 004343 (b.g.) 044727 (b.g.)
046358 O-ring to spray cylinder 044711
Screw to holder 044712
Cover to product collection vessel 046318
Resistant O-ring set in FFKM 046364
Plastic closure for product collection 046358
vessel
Set of peristaltic rolls 046311
10.3 Filters
10.5 Trolley
Trolley 041257
For the precise determination of the gas flow in absolute measures. A pipe generates a laminar flow
for the determination with a hot-wire instrument. The appropriate instrument can be supplied by Testo
(www.testo.com) type Test 435 with sensor No. 0635 1044.
Table 10-18: Measurement tube
Description Order number
gas flow
For safe and automated switching between pure solvent and product when starting and ending the
spray drying process.
Table 10-19: Feed switch valve
044725 Description Order number
046304 Feed switch valve 044725
Y-piece connector 046304
Metal tube connector 004251
004251
With the cylinder insulation the process is carried out with less product loss, closer to scale-up condi-
tions, and more energy-efficient.
Table 10-23: Cylinder insulation
Description Order number
044629
004139
004133
046557
004222
044782
040163
045519
042655
043366
010804
044433
044425
044435
044424
044423
044434
044432 048891
a i
b f
j
k
g
d h
a Nozzle set 1.4 mm titanium cpl. 11056415 f Glass assembly acid resistant 11056386
Nozzle set 2.0 mm titanium cpl. 11056416 complete
b Outlet filter acid resistant cpl. 11056333 g Spray cylinder holder PFA 11056324
coated
c Cyclone metall cover PFA coated 11056327 Knurled screws PFA coated 11056325
d Sensor support adapter 11056318 h Two-fluid nozzle acid resistant 11056320
Clamp ring ID 8 mm 11056387 Three-fluid nozzle acid resist. 11056971
O-ring of fluoroelastomer 7×1.5 mm 004223 i Filter body PFA coated 11056335
Temperature sensor acid resistant 11056329 j Flange coupling PFA coated 11056326
e Needle 0.7 mm titanium 11056415 k Connecting nipple PFA coated 11056328
Nozzle tip 0.7 mm titanium 11056317 Connecting piece PFA coated 11056334
Nozzle cap 1.5 mm titanium 11057509 PTFE Seal SVL 42 003575
Needle 1.4 mm titanium 11056417 l FEP hose ID 6×1 mm 027900
Nozzle tip 1.4 mm titanium 11056419 n.a. O-ring set FFKM 046364
Nozzle cap 2.2 mm titanium 11057510
Needle 2.0 mm titanium 11056422
Nozzle tip 2.0 mm titanium 11056424
Nozzle cap 2.8 mm titanium 11057511
English:
This equipment has been tested and found to comply with the limits for a Class A digital device,
pursuant to both Part 15 of the FCC Rules and the radio interference regulations of the Canadian
Department of Communications. These limits are designed to provide reasonable protection against
harmful interference when the equipment is operated in a commercial environment.
This equipment generates, uses and can radiate radio frequency energy and, if not installed and used
in accordance with the instruction manual, may cause harmful interference to radio communications.
Operation of this equipment in a residential area is likely to cause harmful interference in which case
the user will be required to correct the interference at his own expense.
Français:
Cet appareil a été testé et s’est avéré conforme aux limites prévues pour les appareils numériques
de classe A et à la partie 15 des réglementations FCC ainsi qu’à la réglementation des interférences
radio du Canadian Department of Communications. Ces limites sont destinées à fournir une protec-
tion adéquate contre les interférences néfastes lorsque l’appareil est utilisé dans un environnement
commercial.
Cet appareil génère, utilise et peut irradier une énergie à fréquence radioélectrique, il est en outre
susceptible d’engendrer des interférences avec les communications radio, s’il n’est pas installé et
utilisé conformément aux instructions du mode d’emploi. L’utilisation de cet appareil dans les zones
résidentielles peut causer des interférences néfastes, auquel cas l’exploitant sera amené à prendre les
dispositions utiles pour palier aux interférences à ses propres frais.
BÜCHI Labortechnik AG BÜCHI Labortechnik GmbH BUCHI Sarl BÜCHI Labortechnik GmbH
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T +82 2 6718 7500 Selangor T +65 6565 1175 T +66 2 862 08 51
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