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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
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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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B-290 Operation Manual, Version G

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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55

B-290 Operation Manual, Version G

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)

B-290 Operation Manual, Version G

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.

B-290 Operation Manual, Version G

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.

B-290 Operation Manual, Version G

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.

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

Inert Loop B-295 50 Hz, 230 V

44701

Inert Loop B-295 60 Hz, 200 V

46345

Inert Loop B-295 60 Hz, 230 V

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

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B-290 Operation Manual, Version G

Technical data

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


Mini Spray Dryer B-290

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

Dimensions (W x H x D)

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

Dimensions (W x H x D)

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

B-290 Operation Manual, Version G

Description of function

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.

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B-290 Operation Manual, Version G

Description of function

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
Mini Spray Dryer B-290
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.

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B-290 Operation Manual, Version G

4.5

Description of function

Adsorption unit
Mini Spray Dryer B-290

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
Mini Spray Dryer B-290

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

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B-290 Operation Manual, Version G

Description of function

Dehumidier B-296

Mini Spray Dryer B-290


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.

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B-290 Operation Manual, Version G

4.7

Description of function

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

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B-290 Operation Manual, Version G

4.8.1

Description of function

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
%
%

B-290 Operation Manual, Version G

Putting into operation

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.

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B-290 Operation Manual, Version G

5.3

Putting into operation

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

B-290 Operation Manual, Version G

5.4

Putting into operation

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

B-290 Operation Manual, Version G

Putting into operation

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

B-290 Operation Manual, Version G

5.6

Installing the lters

5.6.1

Outlet lter

Putting into operation

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

B-290 Operation Manual, Version G

5.7

Putting into operation

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

B-290 Operation Manual, Version G

5.8

Putting into operation

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

B-290 Operation Manual, Version G

5.9

Putting into operation

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

B-290 Operation Manual, Version G

5.10

Putting into operation

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

B-290 Operation Manual, Version G

Putting into operation

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

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B-290 Operation Manual, Version G

Putting into operation

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)

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B-290 Operation Manual, Version G

5.13

Putting into operation

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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.

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B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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.

B-290 Operation Manual, Version G

Maintenance and repairs

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

B-290 Operation Manual, Version G

7.5

Maintenance and repairs

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

B-290 Operation Manual, Version G

7.9

Maintenance and repairs

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

B-290 Operation Manual, Version G

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

Defective sensor, sensor cable or


internal wiring

Contact the Buchi customer service

003

Entry temperature excessively high (> 230 C)

Defective heating control or heating


relay

Contact the Buchi customer service

004

Exit temperature sensor


interruption

Defective sensor, sensor cable or


internal wiring

Contact the Buchi customer service

005

Exit temperature sensor


short-circuit

Defective sensor, sensor cable or


internal wiring

Contact the Buchi customer service

006

Exit temperature excessively high

Defective sensor, sensor cable or


internal wiring

Contact the Buchi customer service

010

Malfunction of frequency
converter

Defective frequency converter or wiring

Contact the Buchi customer service

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


Contact the Buchi customer service

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B-290 Operation Manual, Version G

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

Contact the Buchi customer service

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)


Contact the Buchi customer service
Check tubing system

Open compressed air valve


Inspect pressure of air in the supply
tube (5 - 8 bar)

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

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B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

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

B-290 Operation Manual, Version G

BCHI Labortechnik AG
CH-9230 Flawil 1 / Switzerland
T +41 71 394 63 63
F +41 71 394 65 65

www.buchi.com

093001

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