Manual de Operación Mini Sapray Dryer b290

Operation Manual
Mini Spray Dryer
B-290
93001 en
Table of contents
Table of contents
1
2
About this manual . . . . . . . . . . . . . . . . . . . . . .

Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.1
User qualication . . . . . . . . . . . . . . . . . . .
2.2
Proper use . . . . . . . . . . . . . . . . . . . . . .
2.3
Improper use . . . . . . . . . . . . . . . . . . . . .
2.4
Warning notices used in this manual . . . . . . . . .
2.5
Product safety. . . . . . . . . . . . . . . . . . . . .
2.5.1 Instrument-related hazards . . . . . . . . . . . . . .
2.5.2 Other hazards . . . . . . . . . . . . . . . . . . . . .
2.5.3 Safety measures . . . . . . . . . . . . . . . . . . .
2.5.4 Safety elements and measures . . . . . . . . . . . .
2.6
General safety rules . . . . . . . . . . . . . . . . . .
Technical data . . . . . . . . . . . . . . . . . . . . . . . .
3.1
Scope of delivery . . . . . . . . . . . . . . . . . . .
3.1.1 Standard instrument. . . . . . . . . . . . . . . . . .
3.1.2 Standard accessories . . . . . . . . . . . . . . . . .
3.1.3 Standard accessories with the B-290 Advanced . . .
3.1.4 Optional accessories . . . . . . . . . . . . . . . . .
3.2
Technical data overview . . . . . . . . . . . . . . . .
3.3
Materials used. . . . . . . . . . . . . . . . . . . . .
Description of function . . . . . . . . . . . . . . . . . . .
4.1
Functional principle of the drying air . . . . . . . . . .
4.2
Functional principle of the sample feed and dispersion
4.3
Outlet lter. . . . . . . . . . . . . . . . . . . . . . .
4.4
Inert Loop . . . . . . . . . . . . . . . . . . . . . . .
4.5
Adsorption unit . . . . . . . . . . . . . . . . . . . .
4.6
Dehumidier B-296 . . . . . . . . . . . . . . . . . .
4.7
Spray chilling accessory . . . . . . . . . . . . . . . .
4.8
Connected accessories to the Mini Spray Dryer B-290
4.8.1 Feed switch valve and remote control panel . . . . . .
4.8.2 Printer or PC for data output via RS-232 serial port . .
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.6
.7
.7
.7
.7
.8
.8
.8
.9
.9
.9
10
11
11
11
12
12
13
13
14
15
15
15
16
16
17
17
19
19
20
20
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 modications may be made to the instrument without the prior written agreement of
Buchi. Unauthorized modications may affect the system safety or result in accidents.
This manual is copyright. Information from it may not be reproduced, distributed, or used for competitive purposes, nor made available to third parties. The manufacture of any component with the aid of
this manual without prior written agreement is also prohibited.
If you need another language version of this manual, you can download it at
www.buchi.com.
B-290 Operation Manual, Version G
Table of contents
Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

5.1
Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.2
Electrical connections . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.3
Installing the compressed air maintenance unit and compressor (optional)
5.4
Installing the glass assembly . . . . . . . . . . . . . . . . . . . . . . .
5.5
Installing the spraying nozzle . . . . . . . . . . . . . . . . . . . . . . .
5.6
Installing the lters . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.6.1 Outlet lter. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.6.2 Inlet lter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.7
Adjusting the peristaltic pump bed and choosing the feeding tube . . . .
5.8
Tubing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.9
Installing the Inert Loop B-295 . . . . . . . . . . . . . . . . . . . . . .
5.10 Installing the adsorption unit. . . . . . . . . . . . . . . . . . . . . . . .
5.11 Installing the Dehumidier B-296 . . . . . . . . . . . . . . . . . . . . .
5.12 Installing the Spray Chilling Accessory. . . . . . . . . . . . . . . . . . .
5.13 Installation check . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
6.1
Layout of the operating and display elements . . . . . . . . . . . . . . .
6.2
Conversion tables for the parameters . . . . . . . . . . . . . . . . . . .
6.2.1 Flow meter spraying air (rotameter) . . . . . . . . . . . . . . . . . . . .
6.2.2 Peristaltic pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
6.2.3 Aspirator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
6.3
Spray process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
6.4
Optimizing parameters . . . . . . . . . . . . . . . . . . . . . . . . . .
6.5
End of spray process . . . . . . . . . . . . . . . . . . . . . . . . . . .
6.6
Recovering particles of the outlet lter . . . . . . . . . . . . . . . . . . .
6.7
Operation with the Inert Loop B-295 . . . . . . . . . . . . . . . . . . .
6.7.1 Status messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
6.8
Operation with the adsorption unit (optional). . . . . . . . . . . . . . . .
6.9
Operation with the Spray Chilling Accessory. . . . . . . . . . . . . . . .
Maintenance and repairs . . . . . . . . . . . . . . . . . . . . . . . . . . . .
7.1
Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
7.2
Glass assembly, tubes. . . . . . . . . . . . . . . . . . . . . . . . . . .
7.3
Nozzles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
7.4
Inert Loop B-295 and Dehumidier B-296. . . . . . . . . . . . . . . . .
7.5
Outlet lter. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
7.6
Calibrating the oxygen sensor . . . . . . . . . . . . . . . . . . . . . . .
7.7
Replacing the oxygen sensor . . . . . . . . . . . . . . . . . . . . . . .
7.8
Spray chilling accessory . . . . . . . . . . . . . . . . . . . . . . . . . .
7.9
Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
8.1
Error messages and their remedy . . . . . . . . . . . . . . . . . . . . .
8.2
Malfunctions and their remedy. . . . . . . . . . . . . . . . . . . . . . .
Shutdown, storage, transport and disposal . . . . . . . . . . . . . . . . . .
9.1
Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . .
9.2
Disposal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
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21
21
21
22
23
24
25
25
25
26
27
28
29
29
30
32
33
33
34
34
34
35
35
35
36
36
37
38
38
39
40
40
40
40
40
41
41
41
41
42
43
43
44
46
46
46
Table of contents
10
11
Spare parts. . . . . . . . . . . . . . . . . . . .
10.1 Spray nozzle . . . . . . . . . . . . . . .
10.2 Glass parts . . . . . . . . . . . . . . . .
10.3 Filters . . . . . . . . . . . . . . . . . . .
10.4 Tubing. . . . . . . . . . . . . . . . . . .
10.5 Trolley . . . . . . . . . . . . . . . . . . .
10.6 Measurement pipe for gas ow . . . . . .
10.7 Feed switch valve . . . . . . . . . . . . .
10.8 Remote control panel . . . . . . . . . . .
10.9 Inert Loop B-295 and Dehumidier B-296.
10.10 Cylinder insulation . . . . . . . . . . . . .
Declarations and requirements. . . . . . . . .
11.1 FCC requirements (for USA and Canada) .
11.2 Declaration of conformity . . . . . . . . .
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47
47
49
50
51
51
52
52
53
53
53
54
54
55
About this manual
About this manual

This manual describes the Mini Spray Dryer 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.
NOTE
The symbols pertaining to safety (WARNINGS and ATTENTIONS) are explained in chapter 2.
Abbreviations
EPDM: Ethylene Propylene Dimonomer
FFKM: Peruoroelastomers
FPM: Fluoroelastomer
PEEK: Polyetheretherketone
PTFE: Polytetrauoroethylene (Teon)
Safety
Safety
This chapter points out the safety concept of the instrument and contains general rules of behavior
and warnings from hazards concerning the use of the product.
The safety of users and personnel can only be ensured if these safety instructions and the safetyrelated warnings in the individual chapters are strictly observed and followed. Therefore, the manual
must always be available to all persons performing the tasks described herein.
2.1
User qualication
The instrument may only be used by laboratory personnel and other persons who on account of
training or professional experience have an overview of the dangers which can develop when
operating the instrument.
Personnel without this training or persons who are currently being trained require careful instruction.
The present Operation Manual serves as the basis for this.
2.2
Proper use
The instrument has been designed and built as laboratory instrument. It serves to dry aqueous solutions or suspensions in one operating process. In combination with the B-295, it is possible to work
with organic solvents.
If the instrument is used with toxic or hazardous substances, it has to be installed inside a closed fume
cupboard.
2.3
Improper use
Applications not mentioned above are improper. Also, applications which do not comply with the technical data are considered improper. In particular no gases with unknown chemical composition may
be drawn off.
The operator bears the sole risk for any damages caused by such improper use.
The following uses are expressly forbidden:
Spray drying of organic solvents without the Inert Loop B-295 in open cycle.
Use of the instrument in rooms which require ex-protected instruments.
Use on samples which can explode or iname (example: explosives, etc.) due to shock, friction,
heat or spark formation.
Use on oxygen-producing substances.
2.4
Safety
Warning notices used in this manual

WARNING
Generally, the triangular warning symbol indicates the possibility of personal injury or even loss of life
if the instructions are not followed.
WARNING
Electrical hazard.
WARNING
Hot surface.
WARNING
Biohazard.
ATTENTION
With the general Read this symbol, ATTENTION indicates the possibility of equipment damage,
malfunctions or incorrect process results, if instructions are not followed.
NOTE
Useful tips for the easy operation of the instrument.
2.5
Product safety
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 insufciently trained personnel.
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 dangers.
2.5.1
Instrument-related hazards
Pay attention to the following safety notices:
ATTENTION
Risk of instrument damage when the instrument is operated with bent hoses.
Always inspect the instrument for bends or kinks in hoses and eliminate them prior to operation.
2.5.2
Safety
Other hazards
WARNING
Certain gases in or in the vicinity of the instrument are highly inammable.
Always be aware of the explosion risk when working with hazardous substances or with
substances of unknown composition.
Always provide a good ventilation within or in the vicinity of the system.
WARNING
Certain powdery products released when emptying the product collection vessel might be
hazardous.
Protect yourself against contact with those products.
2.5.3
Safety measures
Always wear personal protective equipment such as protective eye goggles, protective clothing and
gloves when working with the instrument.
2.5.4
Safety elements and measures

To arrest electrostatic charges from the instrument, it is internally grounded. There is also the possibility to arrest electrostatic charges from both the product collection vessel and the cyclone.
Heating
Excess temperature protection against uncontrolled overheating.
Automatic temperature control of the inlet temperature.
Air
The system can be used in the suction mode or in the blowing mode. The suction mode is standard
when working with aqueous solutions. 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 intake lter
and aspirator lter, a contamination of the environment through leaking from the instrument. The
blowing mode is used when working with the Inert Loop B-295 to have a small overpressure in the
system. This pressure is a safety element and is indicated to detect a leakage.
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.
Screwing glass connections to prevent glass breakage.
2.6
Safety
General safety rules

Responsibility of the operator
The head of laboratory is responsible for training his 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.
Duty of maintenance and care
The operator is responsible for ensuring that the instrument is operated in proper condition only, and
that maintenance, service, and repair jobs are performed with care and on schedule, and 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 modications to the spare parts used are only allowed with the prior
written permission of the manufacturer.
Modications
Modications to the instrument are only permitted after prior consultation with and with the written
approval of the manufacturer. Modications and upgrades shall only be carried out by an authorized
Buchi technical engineer. The manufacturer will decline any claim resulting from unauthorized modications.
10
Technical data
Technical data
This chapter introduces the reader to the instrument specications. It contains the scope of delivery,
technical data, requirements and performance data.
3.1
Scope of delivery
Check the scope of delivery according to the order number.
NOTE
For detailed information on the listed products, see www.buchi.com or contact your local dealer.
3.1.1
Standard instrument
Table 3-1: Standard instrument
11
Product
Order number
Mini Spray Dryer B-290 200 V
44781
Mini Spray Dryer B-290 230 V
44780
Mini Spray Dryer B-290 Advanced 200 V
44700
Mini Spray Dryer B-290 Advanced 230 V
44699
3.1.2
Technical data
Standard accessories
Table 3-2: Standard accessories
Product
Order number
Operation Manual:
3.1.3
German
93000
English
93001
French
93002
Italian
93003
Spanish
93004
Glass assembly complete
44680
Compressed gas tube, 5 m with quick

coupling, complete
46356
Silicone tube for nozzle cooling, 4 m
04139
Silicone tube (per m)
04138
Cleaning brush for nozzle
44782
Polypress tube for gas stream, 3 m
46341
Hose clamps
04236
Standard accessories with the B-290 Advanced

Table 3-3: Standard accessories with the B-290
Advanced
12
Product
Order number
Lamella safety curtain
44783
Feed switch valve
44725
Spray cylinder, vertical outlet
44697
Nozzle cap, 1.4 mm
44649
Tygon tube MH 2075 transparent (per m)
46314
Tygon tube F 4040 A yellow (per m)
46315
3.1.4
Technical data
Optional accessories
Table 3-4: Optional accessories
3.2
Product
Order number
Inert Loop B-295 50 Hz, 200 V
44779
44701
46345
46344
Dehumidier B-296 50/60 Hz
40188
Spray chilling accessory complete
40351
Adsorption unit, complete
46560
Brown glass assembly
44758
Nozzle, complete
44698
Outlet lter, complete
44754
Inlet lter
11235
Compressed air maintenance unit
04366
Oil-free compressed air supply
27907
Technical data overview

Table 3-5: Technical data Mini Spray Dryer B-290
Mini Spray Dryer B-290
Power consumption
max. 2900 W
Connection voltage
200-230 V 10 %
Frequency
50/60 Hz
Environmental conditions
Temperature
Altitude
Humidity
for indoor use only

5 - 35 C
up to 2000 m
maximum relative humidity 80 % for temperatures up to
31 C decreasing linearly to 67 % relative humidity at
35 C
Evaporating capacity
1.0 l/h H2O, higher for organic solvents
Airow
max. of 35 m3/h
Motor control
Frequency converter
Max. temperature input
220 C
Heating capacity
2300 W
Heating control
PT-100, fuzzy logic, control accuracy 2 C
Interface
Serial port RS-232 for all parameters
Spray gas
Compressed air or nitrogen / 200 - 800 l/h, 5 - 8 bar
Nozzle tip diameter
0.7 mm standard, other sizes 1.4 and 2.0 mm available
Possible particle diameter range
1 - 25 m
Mean residence time
1.0 - 1.5 sec.
Pollution degree
Installation category
II
13
Technical data
Table 3-5: Technical data Mini Spray Dryer B-290 (cont.)

Dimensions (W x H x D)
65 x 110 x 70 cm
Weight
46 kg
Table 3-6: Technical data Inert Loop B-295

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
60 x 70 x 84.5 cm
Weight
95 kg
Table 3-7: Technical data Dehumidier B-296

Dehumidier B-296
3.3
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
35 x 40 x 60 cm
Weight
36 kg
Materials used
Table 3-8: Materials used
Component
Material designation
Glass assembly
3.3 borosilicate glass
Nozzle / heater / connection piece
Stainless steel
Seal of product collection vessel
FPM (FFKM)
Seal cyclone / cylinder
Silicone
Preheat exchanger Inert Loop B-295
Stainless steel
Polypress tube
EPDM
Product feed tube
Silicone and tygon
Molecular sieve bag of adsorption unit
PEEK
14
Material code
1.4301 / 1.4305
1.4301
Description of function
This chapter explains the basic principle of the instrument, shows how it is structured and gives a
functional description of the assemblies.
4.1
Functional principle of the drying air

The Mini Spray Dryer B-290 operates according to a co-current air and product stream. This means
that sprayed product and hot air have the same ow direction.
2
3
1
4
/ Air inlet (optional with attached inlet lter)

0 Electric heater
1 Concentric inlet of the hot air around the
spray nozzle
2 Spray cylinder
3 Cyclone to separate particles from gas
stream
4Product collection vessel
5 Outlet lter
6 Aspirator to pump air through system
6
Fig. 4.1: Functional principle of the drying air
4.2
Functional principle of the sample feed and dispersion

The Mini Spray Dryer has a integrated two-uid nozzle: Compressed air is used to disperse the liquid
body into ne droplets which are subsequently dried in the cylinder.
/ Feed solution
0 Peristaltic pump
1 Two uid nozzle
2 Connection for cooling water
3Connection for compressed air
4Automatic nozzle cleaning system
4
6
3
1
Fig. 4.2: Functional principle of the sample feed and dispersion
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 uid 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.
15
The smaller nozzle cap of 1.4 mm diameter leads to a lower consumption of 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.
4.3
Outlet lter
The outlet lter, consisting of a polyester textile, prevents environmental pollution and the possible
corrosion of the aspirator by very ne particles which cannot be separated in the cyclone. It can be
washed by hand or machine. All needed connections are included.
The second lter included is made of a PTFE membrane. By counter-pulsing the lter 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 lter. With a clean lter, the corresponding
pressure drop is marked.
4.4
Inert Loop
N2
Inert Loop B-295

5
1
6
7
/ Feed
0 Product
1 Exhaust gas
2 Solvent
3 Preheat exchanger
4 Condensation
5 Cooling unit
Fig. 4.3: Combined system of the B-290 and B-295
The Inert Loop B-295 is an accessory to enable the safe use of organic solvent in a closed loop.
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 ows back to the Mini Spray Dryer.
16
4.5
Adsorption unit
Inert Loop B-295
N2
1
3
/Feed
0Product
1Adsorption column
2 Exhaust gas
3 Solvent
Fig. 4.4: Adsorption unit
If mixtures of organic solvents and water are used, we strongly recommend the additional adsorption column in the closed loop system. The separation prevents water from freezing in the Inert Loop
B-295 and potentially damaging the preheat exchanger. The humidity is detected by a sensor. As
soon as a critical threshold is exceeded as the column is saturated, the feed pump is stopped and the
molecular sieve has to be exchanged or regenerated.
4.6
Dehumidier B-296
Dehumidier B-296
8
7
1
4
/Ambient air
0Condensation
1Cooling unit
2 Condensed water
5
3 Product
4Exhaust gas
5Compressed air
6Feed
Fig. 4.5: Open loop Mini Spray Dryer B-290 with Dehumidier B-296 inlet air conditioning
17
Dehumidier B-296

N2
5
1
6
7
2
3 4
/Feed
0Product
1Exhaust gas
2 Condensate
3 External preheat exchanger

4Condensation
5Cooling unit
Fig. 4.6: Dehumidier B-296 used in the closed mode
Use as inlet air conditioning

The Dehumidier B-296 is an accessory to enable a drying under constant and reproducible humidity
conditions cooling to a dew point of 3 - 5 C.
The drying air is passing the refrigerator of the Dehumidier B-296. The humidity in the ambient air
condenses in the refrigerator and is collected in a closed bottle.
The dry air is then heated up by the heater of the B-290.
Use in the closed mode
The Dehumidier B-296 is an accessory to enable the safe use of a water-organic solvent mixture in a
closed loop with up to 50 % organic solvents content.
The inert gas is loaded with water-solvent mixture from the spray drying process in an external preheat
exchanger.
The gas stream from the spray dryer is cooled down in a preheat exchanger (see Fig. 5.15).
The solvent condenses in the Dehumidier B-296 and is collected in a receiving vessel. The cleaned
gas stream ows back and is heated up in the preheat exchanger.
18
4.7
Spray chilling accessory

When a melting is dispersed into a cold gas stream, the droplets are solidied into particles and can
thus be 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).
/ Temperature sensor
0 Circulating heating liquid to bath nozzle - peristaltic pump - bath
1 Cold gas
2 Heated feed sample
1
4
3
Fig. 4.7: Functional principle of the sample feed and dispersion
4.8
Connected accessories to the Mini Spray Dryer B-290
/ Serial port RS-232 for data output to a PC

0 Connection for the remote control panel
1 Connection for Inert Loop B-295
2 Connection for feed switch valve
Fig. 4.8: Rear connections of the Mini Spray Dryer B-290
19
4.8.1
Feed switch valve and remote control panel
Fig. 4.9: Feed switch valve and remote control panel
The remote control enables an easy operation even with closed fume hood. The ow meter for the
spraying air is the only parameter which cannot be adjusted via the remote control panel.
The feed switch valve is a useful tool together with the remote control panel. During the start and end
of the spray process, the feeding tube has to be moved from pure solvent to product solution and
vice versa. This can be automated by means of the feed switch valve. A Y-piece is inserted between
peristaltic pump and feed switch valve.
4.8.2
Printer or PC for data output via RS-232 serial port
The Mini Spray Dryer is supplied with a standard protocol for data readout. This is of special importance if the system is qualied 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 dened as follows:
No.
Information
Type
Unit
Time since mains on
integer
Current temperature inlet
integer
Current temperature outlet
integer
Heater on/off
0/1
Set temperature inlet
integer
Aspirator on/off
0/1
Aspirator rotation speed
integer
Pump on/off
0/1
Pump rotation speed
integer
10
Feed switch valve
1/2
11
Connection Inert Loop B-295 no/yes
0/1
12
Oxygen high
0/1
13
Pressure low
0/1
14
Error message
integer
20
C
%
%
Putting into operation

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 immediately to inform the postal company, railway company or transportation company.
Keep the original packaging for future transportation.
5.1
Installation site
Put the instrument on a stable, horizontal base.
ATTENTION
If the instrument is used with organic solvents, the system must be operated in a fume hood or with
the safety curtain mounted. In this case, the Inert Loop must be connected as well.
5.2
Electrical connections
Connect the power plug to the instrument and to the mains supply.
ATTENTION
Make sure that the voltage on the socket corresponds to the voltage given on the type plate of the
instrument.
Always connect the instrument to an earthed socket. External connections and extension cables
must be provided with an earthed conductor lead (3-pole couplings, cable or plug equipment) as the
mains lead has a molded plug, thus avoiding risks due to unobservant defective wiring.
Make sure that no electric sparks form in the instrument or its surroundings as they might damage
the instrument.
21
5.3
Installing the compressed air maintenance unit and compressor (optional)

To ensure the Mini Spray Dryer achieves an optimal atomisation 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 (see Fig. 5.1).
/ Activated charcoal lter
0 Filter
1 Water separator
1
Fig. 5.1: Compressed air maintenance unit
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 required.
WARNING
Certain gases in compressed air bottles are highly inammable.
Make sure that the compressed air bottles contain compressed air only and no inammable
gases.
22
5.4
Installing the glass assembly

WARNING
Beware of damaged or cracked glass parts.
Check the instrument for damaged glassware before taking it into operation and replace damaged
glassware immediately.
To install the spray cylinder, proceed as follows:
1
2
8
7
6
5
Connect the separation ask 2 to the spray

cylinder 1 by closing the screw connection
(SVL 42) tightly.
Screw the connection piece 4 on the cylinder
outlet ange with the left ange screw joint 5.
The connection is sealed with a Viton o-ring.
Screw the seal holder 0on the instrument
using the three knurled screws.
To mount the cylinder on the instrument,
hold the glass in the upper ange around the
nozzle and insert the connection piece into
the support element 6.
Open the xation 3.
Press the glass ange on the above seal.
Push the lever / carefully on the left side, so
that the ange of the cylinder is held rmly.
Close the xation 3.
4
Attach the cyclone 9 together with the
product collection vessel < to the connection
piece 4 with a second ange screw joint 8.
Screw the glass elbow 7 onto the top of the
cyclone.
Connect the grounding cable : to the cover
of the product collection vessel ; and to the
housing to minimize the electrostatic charge
of the powder.
10
11
6
4
12
13
14
23
Connect the outlet temperature sensor =to

the plug in the housing.
Insert the outlet temperature sensor into the
connection piece 4 and screw it in. A metallic
ring and O-ring is inserted to seal the probe.
Close all connections tightly.
15
Fig. 5.2: Installing the glass assembly
5.5
Installing the spraying nozzle

Insert the nozzle into the heater element at
the top of the instrument.
The two uid spraying nozzle has a connection for the feeding tube /, a connection for
the pressurized air or nitrogen 0 and two
connections 1 for an optional cooling/heating
with an external thermostat. The top connection 2 is for the implemented pneumatic
nozzle cleaning: a needle pushes through the
nozzle and prevents clogging.
Fig. 5.3: Installing the spraying nozzle
The three uid nozzle has a second feed supply

3 instead of the nozzle cleaning.
The three uid nozzle has two connections for
two feeding tubes. An external peristaltic pump
has to be mounted for the second feed supply.
Fig. 5.4: Installing the spraying nozzle
24
5.6
Installing the lters
5.6.1
Outlet lter
Fig. 5.5: Installing the outlet lter
Screw the support angle to the bottom side of the panel.

Hang the lter in directly.
Install the connecting tubing between cyclone and lter with an SVL 42.
5.6.2
Inlet lter
Fig. 5.6: Installing the inlet lter
Connect the inlet lter directly to the air inlet of the heater.
25
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.
To adjust the pump bed, proceed as follows:
Insert the tube and close the pump bed.
Put one tube end in water.
Smoothly blow air in the tube with your mouth.
Turn the xation screw with the allen key (see
adjoining gure).
As long as bubbles rise, continue to tighten the
screw.
Exactly at the moment, when no bubbles appear
anymore, the pump bed is correctly adjusted.
Fig. 5.7: Adjusting the pump bed
Choose the feeding tube according to the following table. For short processes, even unsuitable tubes
can be used, as swelling takes some time.
Table 5-1: Choosing the feeding tube
Solvent
Silicone tube
Tygon MH 2075
Tygon F 4040 A
Methanol
suitable
suitable
suitable
Ethanol
suitable
suitable
suitable
Acetone
unsuitable
suitable
unsuitable
Toluoene
unsuitable
unsuitable
suitable
Isopropanol
suitable
suitable
suitable
Chloroform
unsuitable
unsuitable
unsuitable
Dichloro methane
unsuitable
unsuitable
unsuitable
THF
unsuitable
unsuitable
unsuitable
Ethylacetate
unsuitable
suitable
unsuitable
Hexane
unsuitable
unsuitable
suitable
26
5.8
Tubing
Fig. 5.8: Quick coupling rear side
The Mini Spray Dryer B-290 needs compressed gas for the two-uid 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 can be used in an open or closed cycle. The open cycle is set in the suction
mode as a standard. However, if the exhaust is aggressive and could lead to a corrosion of the aspirator, the instrument can also be run in a blowing mode. This mode leads to a higher noise emission.
1
2
/ Tubing between cyclone respectively lter and aspirator

0 Exhaust tube
Fig. 5.9: Open cycle suction mode
/ Exhaust tube of cyclone or lter, respectively

0 Tubing between aspirator and heater
2
1
Fig. 5.10: Open cycle blowing mode
27
5.9
Installing the Inert Loop B-295

The Inert Loop B-295 has wheels and can be placed
next to the Mini Spray Dryer B-290.
Connect the system to the mains supply with the power
cord.
Connect the two instruments with the communication cable to ensure their safe operation. The tubing is
described below.
Fig. 5.11: Inert Loop B-295
The Inert Loop B-295 has a sideward hose connection

for the exhaust gas. Due to the constant feeding with
nitrogen, a certain amount of it is permanently leaving
the system through this outlet tube. If air is sucked in
through the tube, this is an indication that the closed
loop is not tight.
4
2
3
/ Tubing between outlet lter and B-295 inlet

0 Nitrogen inlet tube
1 Tubing between B-295 outlet and aspirator
2Tubing between aspirator and heater
3 Nitrogen outlet tube
1
3
Fig. 5.12: Tubing B-290/B-295, closed cycle mode with Inert Loop B-295
WARNING
Hazardous fumes. The room might be contaminated with solvents.
Always lead the exhaust tube to a fume cupboard or outside.
28
5.10
Installing the adsorption unit

6
1
5
2
3
/Humidity sensor
0 Electronic box
1Tubing between adsorption unit outlet and
B-295 inlet
2Tubing between B-290 outlet and adsorption
unit inlet
3 Holder of adsorption column
4Cooling water connections
5Tubing between B-295 outlet and B-290 inlet
Fig. 5.13: Installing the adsorption unit
Put the holder of the adsorption column 3on the Inert Loop and x it with the adhesive tape.
Connect the Mini Spray Dryer outlet tube 2 with the inlet of the adsorption unit (on the closed side
without sensor /).
Connect the adsorption unit outlet tube 1to the Inert Loop B-295 inlet.
Connect the outlet of the Inert Loop B-295 to the Mini Spray Dryer B-290 5.
Plug in the Inert Loop B-295 connection cable into the electronic box 0 and connect the connection cable of the box with the Mini Spray Dryer.
Connect cooling water 4or a recirculating chiller to the double jacket of the adsorption column.
This cooling is to take up the heat of adsorption on the double jacket.
ATTENTION
If the adsorption column is not cooled, the temperature may exceed the maximum temperature of
the sensor and lead to a sensor failure.
5.11
Installing the Dehumidier B-296

Used as inlet air conditioning system
Place the Dehumidier next to the Mini Spray Dryer and connect it to the mains supply.
Connect the tubing from the outlet of the Dehumidier to the heater of the Mini Spray Dryer.
Fig. 5.14: Tubing between the B-290 and the B-296
29
Used in the closed mode

When mixtures of organic solvents and water (with less than 50% solvents) are used, the use of the
Dehumidier in closed loop is recommendable. Place the Dehumidier next to the Mini Spray Dryer
and connect it to the mains supply.
The cooling temperature is xed to 0 C. We recommend to use a preheat exchanger to increase the
separation performance.
2
/Preheat exchanger to B-296 inlet

0 B-296 outlet to preheat exchanger
1B-290 outlet to preheat exchanger

2 Preheat exchanger to B-290 inlet
Fig. 5.16: Tubing between the preheat exchanger and the B-290
5.12
Installing the Spray Chilling Accessory
6
/ Product feed vessel
0Heating bath
1 Heater
Mount the complete bath 0 on the top of the

Spray Dryer.
Plug in the heater 1 instead of the standard
air heater.
Connect the long temperature sensor 2
instead of the standard outlet temperature
sensor and put it into the holder of the heating
bath.
5
2 Temperature sensor
3 Capillary inlet
4 Capillary outlet
Fig. 5.17: Spray Chilling Accessory
30
1
3
4
4
7
8
5
4
10
4
11
1
5
1
3
5
Apply the tubes 0 to 6 according to the

above gures. The feeding tube is connectable in two ways depending on whether the
nozzle cleaning option is required or not.
Adjust the peristaltic pump bed to the 6 mm
silicone tube.
/ Needle valve for dosage

0Feeding tube with nozzle cleaning option:
Needle valve - nozzle (feed)
1Cleaning gas nozzle: Instrument - nozzle (top)
2 Heating liquid tube: Bath - nozzle (C in) nozzle (C out) - peristaltic pump - bath
3Drain tube for heating liquid
4Gas ow tube: Instrument - capillary inlet

5Gas ow tube: Capillary outlet - nozzle (gas)
6Feeding tube without nozzle cleaning option
7Nozzle cleaning unit
8 Screw connection for feeding tube
9Closed feed connection
Fig. 5.18: Installing the spray chilling tubing with (left) or without nozzle cleaning option (right)
31
5.13
Installation check
Carry out an installation check after a successful installation and prior to the rst 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.
32
Operation
Operation
This chapter gives examples of typical instrument applications and instructions on how to operate the
instrument properly and safely.
WARNING
Risk of injury.
Never operate the instrument when glassware is damaged.
WARNING
Risk of burns when touching the spray cylinder and nozzle during or directly after operation.
Do not touch the spray cylinder or nozzle during operation but let it cool down after operation to
handle it.
6.1
Layout of the operating and display elements

/ Main switch
0 Flow meter for spraying gas volume
1 Needle valve for gas ow adjustment
3
Fig. 6.1: Switch, ow meter and valve
6
1
/ LED display current value inlet air temperature

0LED display current value outlet air temperature
1 LED display set value inlet air temperature
2 LED display aspirator output in % of max. aspirator
rate
3 LED display pump output in % of max. pump rate
4 LED display for nozzle cleaning
5 Feed switch valve button
14
12
10
15
13
11
6 Nozzle cleaner interval adjustment

7 Manual operation pneumatic nozzle cleaner
8 Regulating push-button pump
9 Main switch pump
: Regulating push-button aspirator
; Main switch aspirator
< Regulating push-button heating
= Main switch heating
Fig. 6.2: Operating and display elements
33
6.2
Conversion tables for the parameters
6.2.1
Flow meter spraying air (rotameter)
Operation
The rotameter is an indicator for the spray gas ow. The table gives a correlation between indicated
height and volume throughput. The nozzle has a certain pressure drop which increases with higher
gas ow. As the gas volume strongly corresponds to the actual pressure, the table also contains a row
for the effective volume ow, determined in a spray process with water.
Height (mm)
Liters / hour
Pressure drop (bar)
Actual volume ow (at standard

temperature and pressure)
in liters / hour
6.2.2
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
Peristaltic pump
The peristaltic pump can be adjusted to different tubes according to the inner and outer
diameters. With different tube diameters, the
absolute ow is varying. The diagram shows
the correlation for the standard 2/4 silicone
tube.
Fig. 6.3: Pump settings versus throughput
34
6.2.3
Operation
Aspirator
The aspirator has a maximum gas ow rate
of approx. 35 m3/h. The ow depends on the
pressure drop of the overall system.
To determine the exact volume ow for steady
and reproducible operating conditions, a measur ement tube is supplied as an accessory.
A Testo handheld ow meter (hot-wire ow
meter) is required for the measurement.
Fig. 6.4: Aspirator settings versus throughput
6.3
Spray process
To carry out the spray process, proceed as follows:
1. Switch on the instrument. The instrument carries out an automatic self check and then switches
automatically to the operating mode.
2. Set the air ow to about 30 mm with the rotary switch.
3. Pre-select the desired inlet temperature with the push-button.
4. Turn on the aspirator. As a standard, the aspirator rate should be 100 % to maximize the separation rate of the cyclone. If a small powder humidity is required, the aspirator rate can be
decreased.
5. Turn on the heating and wait until the system has reached steady conditions.
6. If necessary, turn on the nozzle cooling.
7. Switch on the peristaltic pump. Pure solvent, e.g. distilled water in case of aqueous solutions, is
now sprayed in. The spray cone is symmetrical and located in the axis of the spray cylinder. If this
is not the case, the nozzle may be dirty or defective.
8. Set the automatic nozzle cleaning in case of clogging substance.
9. The spray quantity of pure solvent can be changed by means of the push-button of the peristaltic
pump. The spray ow strongly inuences the outlet temperature, since the water draws energy
from the air by evaporation. Thus the outlet temperature can be set to the desired value by means
of the quantity of sprayed solution via the pump speed of the peristaltic pump.
The outlet temperature can be regarded as the upper thermal load of the product, so make sure
that the product is not damaged as a result of an excessively high outlet temperature.
10. As soon as the desired operating conditions have been achieved and are stable, change the feed
tube from pure solvent to the prepared feed solution.
6.4
Optimizing parameters
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
nd the document to download.
35
6.5
Operation
End of spray process

After 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 efcient 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.
6.6
Recovering particles of the outlet lter

If the system is run with a PTFE lter, the ne particles can partially be recovered by counter-pulsating
the lter membrane and blowing the particles away. For this purpose, proceed as follows:
Fig. 6.5: Recovering particles of the outlet lter
Attach the PTFE membrane instead of the polyester lter and close the bottom with a polypropylene plug.
Separate the manometer tube from the lter and remove the lter housing completely from the
holder.
Put the lter on the product feed table. Disconnect the nozzle cleaning tube from the nozzle and
connect it to the lter 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 lter leading to a separation of the nes from the membrane. The particles fall into the
glass and can be recovered.
36
6.7
Operation
Operation with the Inert Loop B-295

ATTENTION
Do not unplug the communication cable between Mini Spray Dryer B-290 and Inert Loop B-295 but
switch off the instruments rst.
ATTENTION
Aqueous solutions or mixtures of organic solutions and water may freeze in the preheat exchanger
of the Inert Loop B-295. Therefore, when working with water or mixtures with organic solvents, the
cooling temperature must be set above +10 C. The use of the adsorption unit is highly recommended when working with water-organic solvent mixtures.
To operate the instruments, proceed as follows:
1. Switch on the Mini Spray Dryer. The instrument automatically detects the connected periphery.
Both signal lamps at the Inert Loop are lit. If the oxygen signal lamp is off, there might still be
enough inert gas in the loop. In this case, open one tube connection wherever possible and let
the aspirator run for 2 minutes, as ambient oxygen concentration is required to check the oxygen
sensor prior to each process.
2. Switch on the aspirator and the heater.
3. Check whether the spray gas source is an inert gas, normally nitrogen. Open the needle valve
at the ow meter and adjust the ow to the requested level. The closed system now starts to be
inertised.
4. As soon as a certain pressure drop threshold is reached by the gas ow and spraying gas, the
signal lamp of the pressure display 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 and the message PR LO on the
display.
5. The overpressure in the system due to the constant ow inlet is limited by the exhaust outlet at the
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 ow 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 goes out. 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 and the message O2 HI on the display.
7. As soon as both signal lamps go out, the peristaltic pump and the heater are deblocked and 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 deblocked again und must be started
manually.
8. At the right bottom side of the Inert Loop B-295 a ask is positioned to receive the condensed
solvent. To empty the ask, close the valve at the top and take out the ask carefully.
37
6.7.1
Operation
Status messages
Table 6-1: Status messages
Code
Description
Possible cause
Corrective measure
O2 HI
O2 sensor indicates excessively high O2 content
Oxygen connected instead of

nitrogen
System not yet sufciently inert
(display on oxygen measurement
equipment still above threshold level
but falling)
Oxygen enters system because of a
leak
Connect nitrogen supply
Leakage in gas circulation system or

clogged lter
Check tubing system (seals in place

and in proper condition, cover rmly
closed) or replace / clean lter
PR LO Pressure monitor shows

operation taking place at too
low pressure
6.8
Wait until threshold level is reached
Check tubing system (seals in place

and in proper condition, cover rmly
closed)
Operation with the adsorption unit (optional)

The molecular sieve is adsorbing the water. The nal humidity is measured with a humidity sensor.
As long as the humidity is below a certain level, the LED on the electronic box is green. When the
humidity starts to rise, the LED changes its color to yellow, but operation is still feasible. As soon as
a critical threshold is exceeded, the red LED is lit and the peristaltic pump, and thus the feeding, is
stopped.
The full load of the molecular sieve bag is approximately 320 g water.
Exchange the molecular sieve bag for a dry one and
continue to work. The molecular sieve bag is regenerated in a vacuum drying oven at 10 mbar or lower
and 150 C (but not more than 200 C). Typically, the
regeneration takes place overnight.
Fig. 6.6: Operation with the adsorption unit
38
6.9
Operation
Operation with the Spray Chilling Accessory

To operate the Spray Chilling Accessory, proceed as follows:
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
39
Fill a heating medium, e.g. water or a thermal oil into the heating bath and check whether the
tubings are connected correctly.
Fill in the product into the product feed vessel. Close it with the glass cover.
Switch on the instrument. Due to the connected long temperature probe, the instrument is preset
to the spray chilling mode.
Set the temperature of the heating bath. A heating temperature 50 % above the melting point of
the product is recommended (e.g. melting point 60 C: heating bath 1.5 x 60 C = 90 C).
Switch on the peristaltic pump with a pump rate of 30 %. Switch on the heater.
Turn on the air ow to approximately 40 mm. The air is preheated in the bath and thus will not
lead to a cooling down of the melt in the nozzle.
Wait for approximately 1 hour until the system is heated up and has steady conditions. The
temperature is displayed as OUTLET temperature.
In case of an optional cooling of the inlet air, switch on the Dehumidier B-296. The Inlet temperature shows the temperature of the cooling air.
Switch on the aspirator. Wait until the complete system has reached steady conditions. Check
that the melt in the product feed vessel is completely liquid.
Open the needle valve. The hot melt will pour into the two uid nozzle. In case of a blocked
nozzle, push the nozzle cleaning.
Wait until all of the product is dispersed.
Switch off the aspirator, the heater, and the peristaltic pump and turn off the spray ow.
Remove the product collection vessel with the powder.
Carefully empty the heating bath at the outlet opening.
Maintenance and repairs

This chapter gives instructions on all maintenance work to be performed in order to keep the instrument in good working condition.
WARNING
Electrical hazard:
Prior to all maintenance work on the instrument switch off the power supply, unplug the instrument, switch off the compressed air and cooling water and remove all sources of ammable
vapor.
ATTENTION
Always wear personal protective equipment such as protective eye goggles, protective clothing and
gloves when maintaining the instrument.
7.1
Housing
Check the housing for defects (switches, plugs) and clean it regularly with a damp cloth.
ATTENTION
Never use solvents as cleaning agents as these might damage the instrument.
7.2
Glass assembly, tubes

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 efcient 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.
7.4
Inert Loop B-295 and Dehumidier B-296

The systems can be ooded completely. For this purpose, raise the exhaust tube and ll the system
with cleaning medium (water or organic solvent).
Provide a collection vessel to collect the cleaning medium owing from the system.
Now open the drain valve and lower the exhaust tube, so that the cleaning medium ows out.
Connect the tube to the Mini Spray Dryer and dry it by running the aspirator.
40
7.5
Outlet lter
If the pressure drop of the outlet lter increases by more than 20 mbar relative to the clean lter, take
the lter out and wash it manually or in a laboratory washing machine or replace it by a new lter.
7.6
Calibrating the oxygen sensor

The oxygen sensor is already calibrated ex works. However, due to shipping and other inuences, the
sensor might have to be calibrated again. At atmospheric condition, it has to display 21.0 1.5%.
1 2
3 4
Remove the front plate with a screwdriver

Open the cover of the buttons on the oxygen analyzer
by turning it in vertical position.
Press menu 2, C:01 will appear.
Press UP 0/ DOWN / to change to C:02.
Press Enter 1, the oxygen concentration is shown on
the display.
Press Enter 1 again to calibrate the sensor.
Press Menu 2 to quit the menu mode.
Fig. 7.1: Calibrating the oxygen sensor
7.7
Replacing the oxygen sensor

After approximately 2 years of operation the 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, Calibrating the oxygen sensor.
Fig. 7.2: Replacing the oxygen sensor
7.8
Spray chilling accessory

Remove the spray chilling accessory after each spray process and clean it e.g. in a heating oven or
with hot water.
41
7.9
Customer service
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 ofcial Buchi customer service ofces are given on the Buchi website under:
www.buchi.com. If malfunctions occur on your instrument or you have technical questions or application problems, contact one of these ofces.
The customer service offers the following:
Spare part delivery
Repairs
Technical advice
42
Troubleshooting
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 ofcial service manuals. In this case, please refer to your local Buchi
customer service agent.
8.1
Error messages and their remedy

Table 8-1: Error messages and their remedy
Code
Description
Possible cause
Corrective measure
001
Entry temperature sensor

interruption
Defective sensor, sensor cable or

internal wiring
Contact the Buchi customer service
002
Entry temperature sensor

short-circuit

internal wiring
003
Entry temperature excessively high (> 230 C)
Defective heating control or heating

relay
004
Exit temperature sensor

interruption

internal wiring
005
Exit temperature sensor

short-circuit

internal wiring
006
Exit temperature excessively high

internal wiring
010
Malfunction of frequency
converter
Defective frequency converter or wiring
011
Heating malfunction
See System does not heat up
See System does not heat up
Only for operation with the Remote Control Panel

100
Connection to Remote
Control Panel interrupted or
disconnected
Defective connection cable or instrument is not plugged in
Check connection cable for

damage and insert plug, if necessary
Only for operation with the Inert Loop B-295

200
Connection to B-295 interrupted or disconnected
Defective connection cable or instrument is not plugged in
Check connection cable for

damage and insert plug, if necessary
201
B-295 plugged in while

operation in process
Connection cable plugged in after

switching on instrument
Restart the system
202
O2 alarm not given during

start-up
Oxygen sensor spent

Oxygen measuring equipment defective
Replace the oxygen sensor

43
Troubleshooting
Table 8-1: Error messages and their remedy (cont.)
8.2
Code
Description
Possible cause
Corrective measure
203
Pressure alarm not given

during start-up
Pressure switch defective or contaminated
204
Humidity sensor above

threshold
Molecular sieve saturated with water
Exchange the molecular sieve bag

and regenerate the used one
Malfunctions and their remedy

Table 8-2: Malfunctions and their remedy
Malfunction
Possible cause
Corrective measure
Equipment cannot be switched on
No voltage
Insert mains plug/examine plug for

damage
Replace the fuse (3.15 A)
Fuse has blown

Peristaltic pump does not deliver
The rollers are not in contact with the

running surface
Elevate the running surface with the

lever
Adjust the lifting height of the running
surface with the hexagonal allen key
from beneath
Product is delivered after the

The pressure of the rollers on the
spray ow is switched on although running surface is too weak
the pump is switched off
Adjust the lifting height of the running

surface with the hexagonal allen key
from beneath
Aspirator is noisy
Clean the aspirator

If no discharge lter is tted, this
should be done to avoid further
contamination of the aspirator
Reset to Suction mode if possible
The aspirator is dirty
The operating mode is set to Blow

System does not heat up
Nozzle blocked up
Heating circuit not plugged in

Heating is not switched on
Nominal entry temperature is below
room temperature
Fuse has blown
Heater defective
Faulty tubing system
(Faulty ow direction or no ow in the
heating system)
Plug in heating circuit

Switch on heating circuit
Pre-select a new inlet temperature
Product is too concentrated
Use a lower concentration in pump

Increase number of pulses for nozzle
cleaning
Cool nozzle with cooling water
Encrustation on nozzle exit

Product drips in spray chamber
44
No spray ow
Insufcient spray ow
Replace fuse (12.5 A)

Check tubing system
Open compressed air valve

Inspect pressure of air in the supply
tube (5 - 8 bar)
Troubleshooting
Table 8-2: Malfunctions and their remedy (cont.)

Malfunction
Possible cause
Corrective measure
Insufcient aspirator performance
Discharge lter blocked
Dismantle lter and clean it
Deposits on the spray cylinder
Nozzle is not clean
Completely dismantle the nozzle and

clean with water
Replace nozzle or defective element
Nozzle is defective (bent nozzle

needle)
Product will not dry
Reduce the temperature difference

between entry and exit
Increase rate of gas spray ow
(> 600 l /h)
Reduce peristaltic pump performance
Entry temperature is above the melting Reduce entry temperature
point of the product
Product related deposits
No action possible
Glass elements become wet
Peristaltic pump lever has become

loose
Tighten lever
Irregular or pulsed spraying
Leaks in the spray nozzle
Check seals in the spray nozzle and

replace if necessary
Deposits in the cyclone
Product related deposits

Static charge build-up
Product too moist
No measure possible
Insert earthing cable
Increase exit temperature to dry the
product
Reduce aspirator performance to
reduce residence time of product
Temperature too high

Exit temperature does not rise
Sensor not inserted

Fault in tubing system
Place probe in coupling element

Check tubing system
Entry temperature falls
Heating is switched off

Heater plug is unplugged
Fuse has blown
Switch on heating
Insert heater plug
Replace fuse (12.5 A)
Exit temperature falls
No heating
Follow measures under Fall of entry

temperature
Reduce production rate of peristaltic
pump
Spraying too powerful

Exit temperature rises
Nozzle blocked
Hose not dipped into stock solution

Change of concentration in stock
solution
No feed of product
45
Clean the nozzle by actuating the

cleaning button or by switching on
cleaning nozzle
Increase number of pulses for the
nozzle cleaning activity
Dip hose into product
Agitate product (magnetic agitator) to
obtain uniform concentration
Switch on peristaltic pump
Shutdown, storage, transport and disposal
Shutdown, storage, transport and disposal

This chapter instructs how to shut down the instrument, how to pack it for storage or transport, and
species the storage and shipping conditions.
9.1
Storage and transport

WARNING
Biohazard:
Remove all dangerous substances from the instrument and clean it thoroughly.
Store the instrument and its accessories at a dry place. Store and transport the instrument in its
original packaging.
WARNING
Due to the weight of the instrument manual handling of the instrument should always be done by two
people.
9.2
Disposal
To dispose of the instrument in an environmentally friendly manner, a list of materials is given in
chapter 3. This helps to ensure that the components are separated and recycled correctly.
Please follow valid regional and local laws concerning disposal.
46
10
10
Spare parts
Spare parts
This chapter lists spare parts, accessories, and options including their ordering information.
Order the spare parts from Buchi. Always state the product designation and the part number when
ordering spare parts.
Use only genuine Buchi consumables and genuine spare parts for maintenance and repair to assure
good system performance and reliability. Any modications to the spare parts used are only allowed
with the prior written permission of the manufacturer.
10.1
Spray nozzle
44629
44628
38024
44643
Table 10-1: Spray nozzle

Description
Order number
Needle for nozzle cleaning
44618
Screw connection product tube
44628
Screw connection air and cooling
44629
Nozzle tip
44634
Nozzle cleaning complete
44643
Nozzle cap 1.5 mm
44647
Nozzle cap 1.4 mm
44649
Set of O-rings
44759
O-ring in Kalrez for nozzle tip
46361
Metallic spring
38024
44634
44618
44647
44649
47
10
Spare parts
Table 10-2: Three uid nozzle

Description
Order number
Three uid nozzle, complete
46555
Three uid nozzle conversion kit
46556
Screw connection product tube
44628
Screw connection air and cooling
44629
Inner nozzle tip 0.7 mm
44554
Nozzle tip 2.0 mm
46377
Nozzle cap 2.8 mm
46375
Set of O-rings
44759
O-ring in Kalrez for nozzle tip
46361
46377
46554
46375
48
10
10.2
Spare parts
Glass parts
Table 10-3: Glass parts 1
46311
44726 (B)
44673
44711
46333
46334 (B)
03551
40674
40162
Description
Order number
Screw cap SVL 42
03551
Separation ask
04188
Cyclone
04189
Seal to cyclone
04192
Separation ask, brown glass
04343
Cyclone, brown glass
04348
Flange screw coupling
34139
Outlet temperature sensor
40162
Seal to product collection vessel
40471
Silicone seal SVL 42
40674
Angle piece
04189
04348 (B) Angle piece, brown glass
Cylinder, sideways outlet
04192
Product collection vessel
04189
34139/
40471
03551
40674
40133
04188
04343 (B)
44678
44727 (B)
46333
46334
44673
44678
O-ring to spray cylinder
44711
Cylinder, sideways outlet, brown glass
44726
Product collection vessel, brown glass
44727
Cover to product collection vessel
46318
Resistant O-ring set in Kalrez
46364
Plastic closure for product collection

vessel
46358
Set of peristaltic rolls
46311
Table 10-4: Glass parts 2
46343
Description
Order number
O-ring
01535
Tension spring
32017
Set ange screw coupling (2 units)
40133
Set O-ring and clamping ring (5 units)
46343
O-ring Kalrez for screw coupling
46363
32017
01535
49
10
Spare parts
Table 10-5: High-performance cyclone

46368
46370
03223
46367
10.3
Description
Order number
High-performance cyclone
46368
Small product collection vessel
46367
Screw ring SVL 30
03223
PTFE seal SVL 30 x 20
05203
Silicone seal 30 x 20
03561
Cyclone complete (all above numbers)
46369
Large product collection vessel
46370
Filters
Table 10-6: Outlet lter
46309
03551
34139
40471
03575
44624
35008/
46316
Description
Order number
Screw cap SVL 42
03551
Seal SVL 42, PTFE
03575
Flange screw coupling
34139
Seal to product collection vessel
40471
Polyester lter bags (6 units)
35004
Polyester lter bag
35008
Filter glass
44624
Filter tube, complete
46309
PTFE membrane lter
46316
Table 10-7: Inlet lter
50
Description
Order number
Inlet lter, complete
11235
Replacement lter with seal
11238
10
10.4
Spare parts
Tubing
03551
04155
46309
44679
04236
46310
04113
46341 (3 m)
46329 (2 m)
46330 (0.6 m)
Table 10-8: Tubing

Description
Order number
Solaex tube
04113
Silicone tube (per m)
04138
ICO quick coupling
04155
Polypress tube (3 m)
46341
Polypress tube (2 m)
46329
Polypress tube (0.6 m)
46330
Filter tube, complete
46309
0.1 m extube PFA
46310
Tygon tube MH 2075 transparent (per m) 46314
10.5
Tygon tube F 4040 A yellow (per m)
46315
Screw cap SVL 42
03551
Tubing nipple
44679
Hose clamp
04236
Tube connector 4 x 2 mm
04251
Trolley
The trolley consists of powder-coated stainless steel.
Dimensions (L x W x H): 850 x 420 x 560 mm
Table 10-9: Trolley
51
Description
Order number
Trolley
41257
10
10.6
Spare parts
Measurement pipe for gas ow

For the precise determination of the gas ow in absolute measures. A pipe generates a laminar ow
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 10-10: Measurement tube
10.7
Description
Order number
Measurement pipe for gas ow
44790
Feed switch valve

For safe and automated switching between pure solvent and product when starting and ending the
spray drying process.
Table 10-11: Feed switch valve
52
Description
Order number
Feed switch valve
44725
10
10.8
Spare parts
Remote control panel

Table 10-12: Remote control panel
10.9
Description
Order number
Remote control panel
44702
Inert Loop B-295 and Dehumidier B-296

Table 10-13: Inert Loop and Dehumidier
46348
04105
Description
Order number
Receiving vessel for solvent
40398
Tube to receiving vessel
04105
PTFE hose connection SVL 22
27338
Oxygen sensor
46348
Adapter piece B-296 for B-190/191
40056
Preheat exchanger
40059
27338
40398
10.10
Cylinder insulation
With the cylinder insulation the process is carried out with less product loss, closer to scale-up conditions, and more energy-efcient.
Table 10-14: Cylinder insulation
53
Description
Order number
Cylinder insulation
40058
11
11
Declarations and requirements
11.1
FCC requirements (for USA and Canada)
Declarations and requirements
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.
Franais:
Cet appareil a t test et s'est avr conforme aux limites prvues pour les appareils numriques
de classe A et la partie 15 des rglementations FCC ainsi qu la rglementation des interfrences
radio du Canadian Department of Communications. Ces limites sont destines fournir une protection adquate contre les interfrences nfastes lorsque lappareil est utilis dans un environnement
commercial.
Cet appareil gnre, utilise et peut irradier une nergie frquence radiolectrique, il est en outre
susceptible dengendrer des interfrences avec les communications radio, sil nest pas install et
utilis conformment aux instructions du mode demploi. Lutilisation de cet appareil dans les zones
rsidentielles peut causer des interfrences nfastes, auquel cas lexploitant sera amen prendre les
dispositions utiles pour palier aux interfrences ses propres frais.
54
BCHI Labortechnik AG
CH-9230 Flawil 1 / Switzerland
T +41 71 394 63 63
F +41 71 394 65 65
www.buchi.com
093001
Quality in your hands

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Operation Manual

Mini Spray Dryer

About this manual . . . . . . . . . . . . . . . . . . . . . .

B-290 Operation Manual, Version G

Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

B-290 Operation Manual, Version G

B-290 Operation Manual, Version G

About this manual

About this manual

B-290 Operation Manual, Version G

B-290 Operation Manual, Version G

Warning notices used in this manual

B-290 Operation Manual, Version G

Safety elements and measures

B-290 Operation Manual, Version G

General safety rules

B-290 Operation Manual, Version G

Mini Spray Dryer B-290 200 V

Mini Spray Dryer B-290 230 V

Mini Spray Dryer B-290 Advanced 200 V

Mini Spray Dryer B-290 Advanced 230 V

B-290 Operation Manual, Version G

Glass assembly complete

Compressed gas tube, 5 m with quick

Silicone tube for nozzle cooling, 4 m

Silicone tube (per m)

Cleaning brush for nozzle

Polypress tube for gas stream, 3 m

Standard accessories with the B-290 Advanced

Lamella safety curtain

Feed switch valve

Spray cylinder, vertical outlet

Nozzle cap, 1.4 mm

Tygon tube MH 2075 transparent (per m)

Tygon tube F 4040 A yellow (per m)

B-290 Operation Manual, Version G

Inert Loop B-295 50 Hz, 200 V

Inert Loop B-295 50 Hz, 230 V

Inert Loop B-295 60 Hz, 200 V

Inert Loop B-295 60 Hz, 230 V

Dehumidier B-296 50/60 Hz

Spray chilling accessory complete

Adsorption unit, complete

Brown glass assembly

Outlet lter, complete

Compressed air maintenance unit

Oil-free compressed air supply

Technical data overview

for indoor use only

1.0 l/h H2O, higher for organic solvents

Max. temperature input

PT-100, fuzzy logic, control accuracy 2 C

Serial port RS-232 for all parameters

Compressed air or nitrogen / 200 - 800 l/h, 5 - 8 bar

Nozzle tip diameter

0.7 mm standard, other sizes 1.4 and 2.0 mm available

Possible particle diameter range

Mean residence time

1.0 - 1.5 sec.

B-290 Operation Manual, Version G

Table 3-5: Technical data Mini Spray Dryer B-290 (cont.)

Table 3-6: Technical data Inert Loop B-295

Min. outlet temperature

Table 3-7: Technical data Dehumidier B-296