BUCHI B-90 User Manual

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Operation Manual

Nano

Spray Dryer B�90

093261

Table of contents

1 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6

2 Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7

2.1 User qualiﬁcation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

2.2 Proper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

2.3 Improper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8

2.4 Safety warnings and safety signals used in this manual . . . . . . . . . . . . . . . . . 8

2.5 Product safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

2.5.1 General hazards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

2.5.2 Warning labels on housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

2.5.3 Safety measures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

2.5.4 Built-in safety elements and measures . . . . . . . . . . . . . . . . . . . . . . . . 14

2.6 General safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

3 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

3.1 Scope of application and delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

3.1.1 Standard instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

3.1.2 Standard accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

3.1.3 Standard accessories with the Nano Spray Dryer B-90 Advanced. . . . . . . . . . . 19

3.1.4 Optional accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

3.2 Technical data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

3.3 Materials used. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

4 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

4.1 Functional principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

4.1.1 Drying gas circuit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

4.1.2 Spray drying process overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26

4.2 Spray generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

4.3 Heating system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

4.4 Drying air generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

4.4.1 Compressed air supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

4.4.2 Aspirator in blowing mode. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

4.5 Sample feed circulation with peristaltic pump . . . . . . . . . . . . . . . . . . . . . 29

4.6 Particle collector. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

4.7 Outlet ﬁlter. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

4.8 Inert Loop B-295 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

4.9 Dehumidiﬁer B-296 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

4.10 Connection at the Nano Spray Dryer B-90 . . . . . . . . . . . . . . . . . . . . . . 33

Read this manual carefully before installing and running your system and note the safety precautions in chapter 2 in particular. Store the manual in the immediate vicinity of the instrument, so that it can be consulted at any time. No technical modiﬁcations may be made to the instrument without the prior written agreement of BUCHI. Unauthorized modiﬁcations may affect the system safety or result in accidents. 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 available versions at www.buchi.com.

3 B-90 Operation Manual, Version B

Table of contents

5 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

5.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

5.2 Installing the Nano Spray Dryer B-90 . . . . . . . . . . . . . . . . . . . . . . . . . 35

5.2.1 Tall set-up with long metal bars . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

5.2.2 Short set-up with short metal bars . . . . . . . . . . . . . . . . . . . . . . . . . . 36

5.3 Sub-assembly installations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

5.3.1 Lifting device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

5.3.2 Electrode assembly installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38

5.3.3 Glass cylinder installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

5.3.4 Heater module installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41

5.4 Spray head assembling and installation . . . . . . . . . . . . . . . . . . . . . . . . 43

5.4.1 Spray head assembling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43

5.4.2 Spray head installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

5.5 Peristaltic pump and feed tubing installation. . . . . . . . . . . . . . . . . . . . . . 47

5.5.1 Peristaltic pump height adjustment and ﬁxation . . . . . . . . . . . . . . . . . . . . 48

5.5.2 Pump bed adjustment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48

5.5.3 Feeding tube installation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49

5.6 Drying gas supply . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51

5.6.1 ‘open loop’ air supply conﬁguration . . . . . . . . . . . . . . . . . . . . . . . . . . 52

5.6.2 ‘closed loop’ gas supply conﬁguration. . . . . . . . . . . . . . . . . . . . . . . . . 53

5.6.3 Outlet ﬁlter installation/replacement . . . . . . . . . . . . . . . . . . . . . . . . . . 53

5.7 Aspirator installation modes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

5.7.1 Aspirator in ‘open loop’ conﬁguration . . . . . . . . . . . . . . . . . . . . . . . . . 54

5.7.2 Aspirator in ‘closed loop’ conﬁguration . . . . . . . . . . . . . . . . . . . . . . . . 55

5.8 Inert Loop B-295 installation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

5.8.1 Main device installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57

5.9 Dehumidiﬁer B-296 installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58

5.9.1 Dehumidiﬁer B-296 in ‘open loop’ conﬁguration . . . . . . . . . . . . . . . . . . . . 59

5.9.2 Dehumidiﬁer B-296 in ‘closed loop’ conﬁguration with out Inert Loop B-295 . . . . . 60

5.9.3 Adsorption column installation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60

5.10 Final installation check. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

5.11 Electrical connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

6 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63

6.1 Starting up the instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63

6.2 Main screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63

6.3 Menu structure overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64

6.4 Display elements and menu functions . . . . . . . . . . . . . . . . . . . . . . . . . 65

6.4.1 Operating controls. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

6.4.2 View parameters menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66

6.4.3 Gas mode selection menu. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67

6.4.4 Conﬁguration menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68

6.4.5 Firmware calibration menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69

6.4.6 Firmware info menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69

6.5 Starting a spray drying process . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70

6.6 Optimizing parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71

6.7 End of spray drying process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72

6.8 Collecting the particles from the collector cylinder . . . . . . . . . . . . . . . . . . . 72

4 B-90 Operation Manual, Version B

Table of contents

6.9 Other operation modes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73

6.9.1 Inert Loop B-295 operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73

6.9.2 Dehumidiﬁer B-296 operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75

6.10 Using the Nano Spray Dryer Records software on a PC. . . . . . . . . . . . . . . . 76

7 Maintenance and repairs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83

7.1 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84

7.2 Housing condition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84

7.3 Glass component conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84

7.4 Oxygen sensor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85

7.5 Sealing conditions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85

7.6 Cleaning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85

7.6.1 Spray head and tube connections. . . . . . . . . . . . . . . . . . . . . . . . . . . 85

7.6.2 Outlet ﬁlter. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86

7.6.3 Inert Loop B-295 and Dehumidiﬁer B-296. . . . . . . . . . . . . . . . . . . . . . . 86

8 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87

8.1 Error messages and their remedy . . . . . . . . . . . . . . . . . . . . . . . . . . . 87

8.2 Malfunctions and their remedy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89

9 Shutdown, storage, transport and disposal . . . . . . . . . . . . . . . . . . . . . . . . 91

9.1 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91

9.2 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92

10 Spare parts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94

10.1 Spray head . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94

10.2 Glass parts and mounting items. . . . . . . . . . . . . . . . . . . . . . . . . . . . 95

10.3 Particle collector, heater and lifting device items . . . . . . . . . . . . . . . . . . . . 96

10.4 Filters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97

10.5 Tubing and accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97

10.6 Inert Loop B-295, Dehumidiﬁer B-296 and Adsorption Column . . . . . . . . . . . . 98

11 Declarations and requirements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .100

11.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . . . .100

11.2 Declaration of conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .101

5 B-90 Operation Manual, Version B

1 About this manual

This manual describes the Nano Spray Dryer B-90 and provides all information required for its safe operation and to maintain it in good working order. It is addressed to laboratory personnel in particular.

Abbreviations

EPDM Ethylene Propylene Dimonomer FFKM Perﬂuoroelastomers FPM Fluoroelastomer PEEK Polyetheretherketone PTFE Polytetraﬂuoroethylene (Teﬂon)

PE Polyethylene PVC Polyvinylchloride

1 About this manual

6 B-90 Operation Manual, Version B

2 Safety

This chapter highlights out the safety concept of the instrument and contains general rules of behavior and warnings from direct and indirect hazards concerning the use of the product. For the users safety, all safety instructions and safety messages in the individual chapters shall be strictly observed and followed. Therefore, the manual must always be available to all persons performing the tasks described herein.

2.1 User qualiﬁcation

The instrument may only be used by laboratory personnel and other persons who on account of training and professional experience know of the potential dangers that can develop when operating the instrument.

Untrained personnel, or persons who are currently being trained, require careful supervision by a qualiﬁed person. The present Operation Manual serves as a basis for training.

2 Safety

2.2 Proper use

The Nano Spray Dryer B-90 and the Nano Spray Dryer B-90 Advanced have been designed and built as laboratory instruments.

• The Nano Spray Dryer B-90 serves to spray-dry aqueous solutions or suspensions in ‘open loop’ with compressed air as drying gas.

• The Nano Spray Dryer B-90 Advanced can additionally process organic solvent solutions or suspensions in ‘closed loop’ when combined with the Inert Loop B-295. Processing in ‘closed loop’ requires N2 or CO2 as an inert gas.

The output particle size of the Nano Spray Dryer B-90 is between 300 nm–5 µm. Thus, the instrument is ideally suited to encapsulate particles and nano particles (<100 nm) from a solution or suspension.

If the instrument is used with potentially toxic or hazardous substances in ‘open loop’, it has to be installed inside a closed fume hood or glove box. In such cases, the complete processing and system handling has to be performed within the ventilated box to avoid toxication and other hazardous situations to the user and the environment.

In any case, all exhausts leaving the exhaust gas tubing have to be lead away instantly by a ventilation system, to remove possibly hazardous substances and fumes from the working area. The ventilation system has to be equipped with safety measures such as outlet ﬁlters to avoid contamination of the environment. When the Nano Spray Dryer B-90 is used in combination with other instruments (e.g.

Aspirator) all related manuals are to be fully observed.

7 B-90 Operation Manual, Version B

2.3 Improper use

Applications not mentioned in section 2.2 are considered to be improper. Applications which do not comply with the technical data (see section 3 of this manual) are also considered to be improper.

The operator bears the sole risk for any damages or hazards caused by improper use!

The following uses are expressly forbidden:

• Use of gases with unknown chemical composition.

• Spray drying of biohazard materials such as viruses or bacteria.

• Spray drying of organic solvents in ‘open loop’ and without the Inert Loop B-295.

• Installation or use of the instrument in rooms, which require ex-protected instruments.

• Spray drying of substances which might explode or ignite due to the processing and the selected

parameters of the Nano Spray Dryer B-90 or installed sub systems.

• Use of samples which might produce oxygen during the processing.

2 Safety

2.4 Safety warnings and safety signals used in this manual

DANGER, WARNING, CAUTION and NOTICE are standardized signal words for identifying levels of hazard seriousness of risks related to personal injury and property damage. All signal words, which are related to personal injury are accompanied by the general safety sign.

For your safety it is important to read and fully understand the below table with the different signal words and their deﬁnitions!

Sign Signal word Deﬁnition Risk level

Indicates a hazardous situation which, if not avoided, will result in death or serious injury.

Indicates a hazardous situation which, if not avoided, could result in death or serious injury.

Indicates a hazardous situation which, if not avoided, may result in minor or moderate injury.

Indicates possible property damage, but no practices related to personal injury.

DANGER

WARNING

CAUTION

NOTICE

★★★★

★★★☆

★★☆☆

★☆☆☆

(property damage only)

Supplementary safety information symbols may be placed in a rectangular panel on the left to the signal word and the supplementary text (see below example).

SIGNAL WORD

Space for

supplementary

safety

information

symbols.

8 B-90 Operation Manual, Version B

Supplementary text, describing the kind and level of hazard / risk seriousness.

• List of measures to avoid the herein described, hazard or hazardous situation.

• ...

2 Safety

Table of supplementary safety information symbols The below reference list incorporates all safety information symbols used in this manual and their

meaning.

Symbol Meaning

General warning

Electrical hazard

Explosive gases, explosive environment

Harmful to life-forms

Hot item, hot surface

Device damage

Inhalation of substances

Pressurized gas/air

Ozone formation

Wear protective mask

9 B-90 Operation Manual, Version B

Wear laboratory coat

Wear protective goggles

Wear protective gloves

Heavy weight, lifting requires more than one person

2 Safety

Additional user information Paragraphs starting with NOTE transport helpful information for working with the device / software or

its supplementaries. NOTEs are not related to any kind of hazard or damage (see example below).

NOTE

Useful tips for the easy operation of the instrument / software.

2.5 Product safety

Safety warnings in this manual (as described in section 2.4) serve to make the user alert and to avoid hazardous situations emanating from residual dangers by giving appropriate counter measures. However, risks to users, property and the environment can arise when the instrument is damaged, used carelessly or improperly.

2.5.1 General hazards

The following safety messages show hazards of general kind which may occur when handling the instrument. The user shall observe all listed counter measures in order to achieve and maintain the lowest possible level of hazard.

Additional warning messages can be found whenever actions and situations described in this manual are related to situational hazards.

10 B-90 Operation Manual, Version B

2 Safety

Danger

Death by suffocation or serious poisoning by inhalation of inert gases.

• Do not inhale inert gases

• Directly withdraw released gases and gaseous substances by sufﬁcient ventilation

• Only operate the instrument in ventilated environments

• Before operation, check all parts, connections and sealings involved in the gasﬂow for proper sealing

• Exchange worn out or defective parts immediately

Danger

Death or serious poisoning by gases or particles due to O2– sensor or ﬁlter malfunction

• Exchange defective O2– sensor immediately

• Exchange O2– sensor regularly within the speciﬁed maintenance intervals

• Exchange clogged ﬁlters immediately

• Exchange ﬁlters regularly within the speciﬁed maintenance intervals

• Dispose of ﬁlter immediately

Danger

Death or serious poisoning by inhalation or incorporation of dried particles during spray process.

• Wear safety goggles

• Wear safety gloves

• Wear a suitable protective mask

• Wear a laboratory coat

• Check for proper sealing before use

• Do not inhale dried particles

• Stop drying gas ﬂow before opening the drying circuit

11 B-90 Operation Manual, Version B

Danger

Death or serious poisoning by inhalation or incorporation of dried particles at recovery.

• Wear safety goggles

• Wear safety gloves

• Wear a suitable protective mask

• Wear a laboratory coat

• Do not inhale dried particles

• Stop drying gas ﬂow before opening the drying circuit

• Only recover particles in sufﬁciently ventilated ﬂue or glove-box

• Do not disperse the dried particles

• Do not clean dusty parts with compressed air

2 Safety

Warning

Death or serious injuries by use in explosive environments.

• Do not operate the instrument in explosive environments

• Do not operate the instrument with explosive gas mixtures

• Before operation, check all gas connections for correct installation

• Directly withdraw released gases and gaseous substances by sufﬁcient ventilation

Warning

Death or serious poisoning by contact or incorporation of harmful substances at use.

• Before operation, check the instrument for correct assembling

• Before operation, inspect sealings and tubes for good condition

• Exchange worn out or defective parts immediately

• Exchange clogged ﬁlters immediately

• Only operate the instrument in ventilated environments

• Directly withdraw released gases and gaseous substances by sufﬁcient ventilation

• Perform a dry-run without sample material and check for gas leakages

12 B-90 Operation Manual, Version B

Caution

Risk of minor poisoning by inhalation of ozone.

• Directly withdraw released gases and gaseous substances by sufﬁcient ventilation

Caution

Risk of minor or moderate burnings when handling hot parts.

• Do not touch hot parts

• Let the system cool down for some minutes after use

2 Safety

Risk of instrument short-circuits and damage by liquids.

• Do not spill liquids over the instrument or its component parts

• Wipe off any liquids instantly

• Place the sample vessel onto the designated reservoir-plate on top of the instrument

• Ensure a safe positioning of the sample vessel

• Do not move the instrument when it is loaded with liquid

• Keep external vibrations away from the instrument

Risk of instrument damage by internal overpressure.

• External supply pressure must meet the system speciﬁcations

• Exchange clogged ﬁlters immediately

• Dispose of ﬁlter immediately

Risk of instrument damage by wrong mains supply.

• External mains supply must meet the voltage given on the type plate

• Check for sufﬁcient grounding

Notice

13 B-90 Operation Manual, Version B

2.5.2 Warning labels on housing

The below warning label can be found at the gas outlet connector on the right side of the Nano Spray Dryer B-90.

Meaning Ozone formation in the electric ﬁeld of the electrostatic particle collector when using oxygen containing

gases as drying gas (like air). Withdraw gases via fume hood or equivalent ventilation system directly.

2 Safety

2.5.3 Safety measures

Always wear personal protective equipment such as protective eye goggles, protective clothing, inhalation protection and gloves when working with the instrument.

2.5.4 Built-in safety elements and measures

Heating

• Overheating protection circuit.

• Automatic temperature control of heater and inlet temperature.

Spraying

• Automatic spray control.

• Light barrier, to detect the correct placement of the particle collector.

• Overpressure leakage detection.

High voltage and electrostatic charges

• Safety current limitation.

• Internal grounding to arrest electrostatic charges.

Air/Gas

• Automatic processing interruption when system pressure is too low.

• Outlet ﬁlter to protect the environment contamination of ﬁne dust particles via exhaust gas tubing.

14 B-90 Operation Manual, Version B

Glass

• High temperature resistance and high transparency borosilicate glass.

Pressure

• Automatic pressure control at outlet ﬁlter.

• Over pressure safety valve (opens at 300 mbar).

Optional system conﬁguration with Inert Loop B-295

• Overpressure leakage detection.

• Safe gas condition (< 6 % O2 content) is detected and enables the regulation of the drying gas mixture via a communication cable.

2.6 General safety rules

Responsibility of the operator The head of the laboratory is responsible for training his/her personnel.

The operator shall inform the manufacturer without delay of any safety-related incidents which might occur during operation of the instrument. Legal regulations, such as local, state and federal laws applying to the instrument must be strictly followed.

2 Safety

Duty of maintenance and care The operator is responsible for the proper condition of instrument at use and that maintenance,

service and repair jobs are performed with care and on schedule by authorized personnel only.

Spare parts to be used Use only genuine consumables and genuine spare parts for maintenance to assure good system

performance and reliability. Any modiﬁcations to the spare parts used are only allowed with the prior written permission of the manufacturer.

Modiﬁcations Modiﬁcations to the instrument are only permitted after prior consultation with and with the written

approval of the manufacturer. Modiﬁcations and upgrades shall only be carried out by an authorized BUCHI technical engineer. The manufacturer will decline any claim resulting from unauthorized modiﬁcations.

15 B-90 Operation Manual, Version B

3 Technical data

This chapter introduces the reader to the instrument and its speciﬁcations. It contains the scope of delivery, technical data, requirements and performance data.

3.1 Scope of application and delivery

The Nano Spray Dryer B-90 is available in two different set-ups:

Nano Spray Dryer B-90 Basic

• For aqueous applications with air in ‘open loop’

Nano Spray Dryer B-90 Advanced

• For solvent applications in combination with Inert Loop B-295

• Optional use with Dehumidiﬁer B-296

• Equipped with additional oxygen safety circuit and gas regulation valves

• Accessories are solvent resistant

3 Technical data

The scope of delivery can only be checked according to the individual delivery note and the listed order numbers.

NOTE

For additional information about the listed products, see www.buchi.com or contact your local dealer.

3.1.1 Standard instrument

Table 3-1: Standard instrument

Product Order no.

Nano Spray Dryer B-90 Basic 50 – 60 Hz, 100 – 240 V

Nano Spray Dryer B-90 Advanced 50 – 60 Hz, 100 – 240 V

11055320

11055321

16 B-90 Operation Manual, Version B

3.1.2 Standard accessories

3 Technical data

Table 3-2: Standard accessories

Product Order no.

Spray head 051510

Spray head holder 051508

Set of 3 spray caps 4.0 µm 051747

Set of 3 spray caps 5.5 µm 051748

Set of 3 spray caps 7.0 µm 051749

HV–Electrode protected 11055174

Protective grid for HV–Electrode 051680

Peristaltic pump complete 051735

17 B-90 Operation Manual, Version B

3 Technical data

Table 3-2: Standard accessories (cont.)

Product Order no.

① Spray cylinder 051511 ② Glass cylinder extension 051549

Glass insulation cylinder (no picture) 051663



Heater complete 051504

Lifting device 051607

«Nano Spray Dryer Records» Software 051776

18 B-90 Operation Manual, Version B

Operation Manual

Nano

Spray Dryer B�90

3 Technical data

Table 3-2: Standard accessories (cont.)

Product Order no.

Outlet ﬁlter 051656

Operation Manual:

English 093261

German 093262

French 093263

Italian 093264

Spanish 093265

093261

Deckblatt B-90_en.indd 1 08.07.2009 09:44:56

3.1.3 Standard accessories with the Nano Spray Dryer B-90 Advanced

Table 3-3: Standard accessories with the B-90

Product Order no.

Oxygen sensor 046348

Tygon tubing MH 2075 transparent (per m) 046314

Tygon tubing F 4040 A yellow (per m) 046315

Upgrade set Nano Spray Dryer B-90 Basic to Advanced

NOTE

Upgrade set is for organic solvent operation in ‘closed loop’ with the Inert Loop B-295 or Dehumidiﬁer B-296. The upgrade set includes solvent resistant tubing, inert gas regulation valves, oxygen sensor with oxygen analyser. The installation requires support of a BUCHI service enginee r.

Advanced (for ‘closed loop’ operation)

11055748

19 B-90 Operation Manual, Version B

3.1.4 Optional accessories

3 Technical data

Table 3-4: Optional accessories

Product Order no.

Inert Loop B-295, 50 Hz, 200 V 044779

Inert Loop B-295, 50 Hz, 230 V 044701

Inert Loop B-295, 60 Hz, 200 V 046345

Inert Loop B-295, 60 Hz, 230 V 046344

Upgrade set B–295 for closed cycle 051783

Dehumidiﬁer B-296, 50/60 Hz, 230 V 040188

Dehumidiﬁer B–296, 50/60 Hz, 200 V 040181

Upgrade set B–296 for closed cycle 051780

Aspirator complete, incl. inlet ﬁlter 051700

20 B-90 Operation Manual, Version B

3 Technical data

Table 3-4: Optional accessories (cont.)

Product Order no.

Inlet ﬁlter 011235

Air maintenance unit 004366

Oil-free air compressor, 230V / 50Hz 027907

Oil-free air compressor, 230V / 60Hz 11055736

Trolley 041257

21 B-90 Operation Manual, Version B

3.2 Technical data

Table 3-5: Technical data Nano Spray Dryer B-90

Power consumption max. 1500 W Connection voltage 100–240 VAC ± 10 %

Input fuse 12 A

Frequency 50 / 60 Hz

Heating capacity max. 1400 W

Max. inlet temperature 120 °C

Evaporating capacity max. 0.2 l/h H2O

Drying gas ﬂow 80–160 l/min

N2 or CO2 inert gas input pressure max. 2 bar

Spray caps (hole diameters) 4.0 µm, 5.5 µm, 7.0 µm

Mean droplet size range 8–21 µm

Mean particle size range 300 nm–5 µm

Mean residence time 1–4 sec.

Interface USB II

IP degree of protection (two digits) IP 42

3 Technical data

Table 3-4: Optional accessories (cont.)

Product Order no.

Stand plate 051775

(higher rates with organic solvents are possible)

Explanation of protection level:

4 Protection provided by the enclosure against access

to hazardous parts (e.g., electrical conductors, moving parts) and the ingress of solid foreign objects with a diameter of > 1mm.

2 Protection of the equipment inside the enclosure

against harmful ingress of dripping water when tilted up to 15°.

Overvoltage category II

Environmental conditions:

Pollution degree 2 (for indoor use only)

Temperature 5–40 °C

Altitude (above sea level) up to 2000 m

Humidity (curve parameter) Maximum relative humidity 80 % up to 31 °C, then

decreasing linearly to 50 % relative humidity at 40 °C

22 B-90 Operation Manual, Version B

Table 3-5: Technical data Nano Spray Dryer B-90 (cont.)

Dimensions (W × H × D)

Short set-up 58×110×55 cm Tall set-up 58×150×55 cm

Weight

Short set-up 65 kg

Tall set-up 70 kg

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

Power consumption max. 1.4 kW

Connection voltage 200–230 V ± 10 %

Frequency 50/60 Hz

Min. outlet temperature down to -25 °C

Rate of cooling 800 W at -10 °C

Dimensions (W×H×D) 60×70×84.5 cm

Weight 95 kg

3 Technical data

Table 3-7: Technical data Dehumidiﬁer B-296

Power consumption 700 W

Connection voltage 200/230 V ± 10 %

Frequency 50/60 Hz

Min. outlet temperature + 2 °C

Rate of cooling 600 W at 0 °C

Dimensions (W×H×D) 35×40×60 cm

Weight 36 kg

Table 3-8: Technical data Aspirator

Power consumption max. 1000 W

Connection voltage 200–240 V ± 10 %

Input fuse FST 5×20 T8A L 250 V

Frequency 50/60 Hz

Dimensions (W×H×D) 47,5×30×32 cm

Weight 20 kg

IP degree of protection (two digits) IP 20

Explanation of protection level:

2 Protection provided by the enclosure against access

to hazardous parts (e.g., electrical conductors, moving parts) and the ingress of solid objects up to 12 mm, e.g. persons ﬁngers.

0 No protection against ingress of liquids.

23 B-90 Operation Manual, Version B

3.3 Materials used

Table 3-9: Materials used

Component Material designation

Glass assembly 3.3 borosilicate glass

Heater Aluminum and stainless steel

Spray head Stainless steel

Spray cap membrane Stainless steel

Spray cap o-ring EPDM75

Feeding tubes Silicone and tygon

Tube connector at feeding tube PEEK

Particle collecting tube Stainless steel polished

HV–electrode Stainless steel

Sealings for spray and glass cylinder Silicone

3 Technical data

24 B-90 Operation Manual, Version B

4 Description of function

This chapter explains the basic working principle of the Nano Spray Dryer B-90 Basic (‘open loop’ only) and the Nano Spray Dryer B-90 Advanced (equipped with O2-sensor and inert gas regulation valves for ‘closed loop’ mode). It also shows how the instruments are structured and provides a general functional description of their assemblies.

4.1 Functional principle

The Nano Spray Dryer B-90 models have been designed to produce particles out of a solution or suspension with a particle size between 0,3 µm–5 µm by drying or encapsulation at a yield rate of up to 90 %. The output particle size depends mainly upon the chosen spray cap. The Nano Spray Dryer B-90 also allows processing of nano particles (<100 nm) in nanosuspensions or emulsions e.g. for encapsulation. The drying gas ﬂow and the product stream are described below.

4.1.1 Drying gas circuit

4 Description of function

The sprayed liquid is accompanied by a co-current gas ﬂow. For highest yields, a controlled gas ﬂow at a sufﬁcient quality and a deﬁned temperature is required. To ensure this, a ﬂow regulator and heating loop has been implemented

a The drying and transport gas enters the instrument

Drying gas inlet

via the “Drying gas inlet”.

b The gas ﬂow is monitored by a “Flow meter”

which inﬂuences the “Gas regulator”.

Gas regulator

Flow meter

Feed pump

c Subsequently the “Electrical heater” heats up the

gas to the desired drying temperature.

Electrical heater

Spray head

d Via the “Inlet temperatur sensor” the heater is

regulated to achieve the desired gas temperature.

Inlet temp. sensor

e The “Relative pressure sensor” compares the in-

ternal to the environmental pressure. In the event of a massive pressure loss (e.g. a leakage) this

safety loop

Drying cylinder

sensor stops the drying process.

f In ‘closed loop’ mode, as part of the safety loop

Electrical particle

collector

the “Oxygen sensor” supervises the percentage of oxygen in the drying gas. In emergency, it stops the process.

Oxygen sensor

Rel. pressure sensor

g The “Outlet temperature sensor” is located after

the particle collector. The temperature drop

Outlet temp. sensor

Outlet ﬁlter

Drying gas outlet

between inlet and outlet temperature sensor is measured as a process value.

h The “Outlet ﬁlter” is a safety relevant item. It re-

tains possibly harmful particles towards the environment in ‘open loop’. In ‘closed loop’ the outlet ﬁlter is an essential part for cleaning the recycled gas from unwanted residues and impurities.

i The “Drying gas outlet” works as an exhaust.

25 B-90 Operation Manual, Version B

Optional drying gas recycling in ‘closed loop’ mode: In ‘closed loop’ mode of the Nano Spray Dryer B-90 Advanced the “Drying gas outlet” i is connected

via the Inert Loop B-295 or Dehumidiﬁer B-296 and Aspirator to the “Drying gas inlet” a.

4.1.2 Spray drying process overview

The drying process takes place inside the drying cylinder. A drying gas ﬂow is established and tiny droplets of sample material are injected by the spray head. The sample material is dried by the hot gas. Because of the tiny particle size, an electrical ﬁeld of sufﬁcient power is needed to retrieve the particulate material from the drying gas ﬂow. The following scheme informs about the different processing stages in general.

Drying gas inlet

Gas regulator

safety loop

Flow meter

Electrical heater

Inlet temp. sensor

Drying cylinder

Electrical particle

collector

Feed pump

Spray head

4 Description of function

a The “Feed pump” constantly feeds the “Spray head”

with liquid sample material.

b The “Spray head” produces ﬁnest droplets and in-

jects them into the “Drying cylinder”.

c The heated drying gas enters laminar from the top

into the “Drying cylinder”. Consequently, the injected drops of sample material are gently dried to solid particles.

d The “Electrical particle collector” retrieves the dried

solid particles by an electrostatic ﬁeld.

e The exhaust gas leaves the spray dryer via the “Out-

let ﬁlter” which retains free particles from the gas.

Oxygen sensor

Rel. pressure sensor

Outlet temp. sensor

Outlet ﬁlter

Drying gas outlet

26 B-90 Operation Manual, Version B

4 Description of function

pull pull

Processing inside the drying cylinder The following draft offers a more detailed view about the basic spray drying process. The drying

gas (a) passes the heater (b) and the vertically or angular aligned spray head (e). The injected micro doplets of the sample material are dried while beeing vortexed in the gas ﬂow inside the spray cylinder (f). An electric ﬁeld is generated by high voltage between the collecting electrode (h) and the HV-electrode (i). While the HV-electrode deﬂects the particulate material, the collecting electrode attracts them. Thus, particles are depositing at the inside of the collecting electrode (g).



















4.2 Spray generation

The Nano Spray Dryer B-90 uses piezotechnology to generate precisely controlled micro droplets from bulk liquids without the use of propellants.















a Drying gas inlet (optional with inlet ﬁlter and Aspira-

tor)

b Electrical heater c Inlet temperature sensor d Display/Control e Spray head (angular or vertical installation) f Spray cylinder and drying section g Finished product at particle collecting electrode h Particle collecting electrode i HV–electrode j Outlet temperature sensor k Outlet ﬁlter l Drying gas outlet (in ‘closed loop’ connected to Inert

Loop B-295 and Aspirator)

push

NOTE

The smaller the mesh size, the smaller the ejected droplets and dried particles. Since the vibrations frequency is ﬁxed, a smaller mesh size will have less throughput per time.

4.3 Heating system

The compact heater module provides optimal energy input to heat the drying gas up to 120 °C. The heating system consists of an electrically heated porous metal foam to minimize the heat–up time and to generate a laminar gas ﬂow towards the drying section. The heating control is based on a pluggable PT–1000 temperature sensor.

push

The spray head includes a piezoelectric actuator with a thin stainless steel membrane. The membrane has an array of micron-sized holes (spray meshes of 4.0,

5.5 or 7.0 µm hole size) and vibrates at ultrasonic frequency (60 kHz). Because of these vibrations the membrane eject precisely sized droplets at high speed.

27 B-90 Operation Manual, Version B

4.4 Drying air generation

In ‘open loop’ mode the required drying air can be either supplied by an in-house compressed air supply, an oil-free compressor or a BUCHI Aspirator (see section 3.1.4, Optional accessories).

4.4.1 Compressed air supply

In ‘open loop’ conﬁguration, compressed air is used as standard drying gas. The air maintenance unit (order no. 004366) is additionally recommended to assure gas of clean, dry and oil free quality. A pressure regulating valve is required to match the instruments input pressure value.

Nano Spray Dryer B-90

Basic

4 Description of function

Air maintenance unit

Product

OUT

a Compressed air source b Optional air maintenance unit c Pressure regulating valve

4.4.2 Aspirator in blowing mode

If there is no compressed air available in the laboratory, the BUCHI Aspirator unit with inlet ﬁlter (order no. 051700) can be used to establish the required drying air ﬂow rate. The Aspirator can be connected directly to the inlet of the Nano Spray Dryer B-90 without a pressure regulating valve. In case of higher ambient humidity use the Dehumidiﬁer B-296 to achieve dry air.

Feed

Control

Outlet filter

Exhaust gas

Compressed

air

b (optional)

NOTE

If the humidity of the air is too high, the current in the particle collector could be too low.

Air inlet ﬁlter The air inlet ﬁlter is required to avoid any contamination of the instruments by ﬁne particles in the lab

environment. It is to be connected to the inlet of the Aspirator, so the instrument aspirates ﬁltered ambient air. The ﬁlter consists of a stainless steel grid for outer protection and an ultra ﬁlter based on a glass ﬁbre textile (ﬁlter class S according to DIN 24184).

28 B-90 Operation Manual, Version B

Nano Spray Dryer B-90

Basic

Feed

Control

Dehumidifier

B-296

COOL

4 Description of function

c (optional)

Aspirator

Product

OUT

a Inlet ﬁlter to ﬁlter out dust and particles b Aspirator as air supply source c Optional Dehumidiﬁer B-296

Condensate

Exhaust gas

Outlet filter

NOTE

The Aspirator is also used with a Nano Spray Dryer B-90 Advanced in ‘closed loop’ conﬁguration with the Inert Loop B-295 or Dehumidiﬁer B-296 to recirculate the inert gas (N2 or CO2).

4.5 Sample feed circulation with peristaltic pump

The peristaltic pump circulates the sample feed between the product vessel and the spray head. It assures a constant substance feeding for the spray generation.

Inlet filter

NOTE

Dry run of the pump and the spray head does not damage the instrument or parts of it in the medium term.

4.6 Particle collector

Solid particles are accumulated at the wall of the cylindrical particle collecting electrode by a strong electrical ﬁeld. The electrical ﬁeld is generated via high voltage.

4.7 Outlet ﬁlter

The outlet ﬁlter (order no. 051656) prevents environmental pollution by particles. It is installed inside the housing of the Nano Spray Dryer B-90. See section 5.5.1 for information about access and exchange.

29 B-90 Operation Manual, Version B

4.8 Inert Loop B-295

The Inert Loop B-295 is an accessory to enable the safe spray drying of organic solvents in a ‘closed loop’ conﬁguration. It comprises a cooling unit with pressure and oxygen monitoring elements and safety controls. Communication to the Nano Spray Dryer B-90 Advanced is established via a communication cable.

Product

4 Description of function

Exhaust gas

COOL

Dehumidiﬁer

a Exhaust gas to fume hood or glove box ventilation

outlet

b Solvent condensate

B-296

c Condensation and cooling unit

Functional principle:

• The inert drying gas (N2 or CO2) is loaded with solvent from the spray drying process.

• The loaded gas enters the Inert Loop B-295 and is cooled down in its internal preheat exchanger.

• The solvent is condensed in the refrigerator and collected in a closed bottle.

• Subsequently, the cleaned and cooled gas stream is heated up in the preheat exchanger and ﬂows back through an Aspirator to the Nano Spray Dryer B-90 Advanced.

Dehumidiﬁer B-296 If mixtures of organic solvents and water are used in ‘closed loop’ conﬁguration, BUCHI strongly

recommends to install the additional Dehumidiﬁer B-296. The Dehumidiﬁer B-296 is condensing the water to prevent water from entering the Inert Loop B-295. This is necessary to protect the heat

exchanger in the refrigerator from water freezing and potential damage.

30 B-90 Operation Manual, Version B

4.9 Dehumidiﬁer B-296

The Dehumidiﬁer B-296 is an accessory which can dry ﬁltered gas at constant and reproducible humidity conditions with a dew point of 3 to 5 °C. The humidity condensates while passing the refrigerator of the Dehumidiﬁer B-296 and is being collected in a closed condensate bottle.

‘open loop’ inlet air conditioning In ‘open loop’ conﬁguration with Aspirator and Inlet ﬁlter the Dehumidiﬁer B-296 has to be connected

to the gas inlet of the Nano Spray Dryer B-90 for inlet air conditioning. The dried, cooled air enters the spray dryer subsequently.

4 Description of function

Nano Spray Dryer B-90

Basic

Feed

Product

OUT

Outlet filter

a Air inlet through ﬁlter b Aspirator in blowing mode c Dehumidiﬁer B-296 to condensate humidity d Dry air output towards Nano Spray Dryer B-90

Control

Dehumidifier

B-296

COOL

Condensate

Exhaust gas

e Condensed water output to collecting ﬂask

Aspirator

Inlet filter

31 B-90 Operation Manual, Version B

4 Description of function

Use in ‘closed loop’ The Dehumidiﬁer B-296 in ‘closed loop’ set-up allows spray drying of water-organic solvent mixtures,

oxygen sensitive substances or ﬂammable powders under safe conditions.

Nano Spray Dryer B-90

Advanced

Product

OUT

Feed

Control

Outlet filter

Dongle

a Inert gas input b Dehumidiﬁer B-296 to condensate humidity c Condensate output to collecting ﬂask

Aspirator

Condensate

Exhaust

gas

Dehumidifier

B-296

Cool

d Aspirator to establish gasﬂow e Dongle to substitute the missing Inert Loop B-295

signals

Suitable spray drying conditions:

• Water-organic solvent mixture with up to 20 % organic solvent content

• For high boiling solvents mixtures (bp > 70 °C) with up to 50 % organic solvent content

In this conﬁguration the used inert gas (N2 or CO2) is loaded with water-solvent mixture residues from the spray drying process. After the cooling and drying process the gas ﬂows back to the spray dryer.

NOTE

To increase the efﬁciency of the dehumidiﬁer signiﬁcantly, it is recommended to use the optional preheat exchanger (order no. 040059). The preheat exchanger also safes energy by heating up the cooled, dehumidiﬁed gas again.

32 B-90 Operation Manual, Version B

4.10 Connection at the Nano Spray Dryer B-90

Front connections

Socket label: Description:

a b c d

a HIGH VOLTAGE Socket for particle collector

b T

c B-295 Inert Loop B-295 communi-

d USB Port for data records to PC

OUT

4 Description of function

with plug thread for reliable plug locking

Outlet temperature sensor socket

cation socket; also used for the dongle to substitute missing communication when operating with Dehumidiﬁer B-296

Rear and side connections

Socket label: Description:

e GAS OUT Gas outlet / exhaust f N

N2 input in ‘closed loop’ mode

g AIR (CO2) Air or CO2 (‘closed loop’) inlet h GAS IN Air inlet in ‘open loop’ mode i Not labelled Gas tube to heater j Not labelled Socket for mains plug k Fuses Resettable fuses l T

Inlet socket for temperature sensor

m HEATER Socket for heater plug

n Pressure relief valve Overpressure safety valve

(opens at a system pressure > 300 m bar)

33 B-90 Operation Manual, Version B

5 Putting into operation

This chapter describes how the instrument has to be installed. It also gives instructions for the 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 surface. Consider the maximum product dimensions and weight. Installation on a mobile trolley is also possible. Obtain the environmental conditions as described in section 3.2, technical data.

5 Putting into operation

NOTE

T o cut the power in case of an emergency by unplugging, the instruments or any other items must

not block the mains plug!

Warning

Death or serious injuries by use in explosive environments.

• Do not operate the instrument in explosive environments

• Do not operate the instrument with explosive gas mixtures

• Before operation, check all gas connections for correct installation

• Directly withdraw released gases and gaseous substances by sufﬁcient ventilation

Caution

Risk of minor or moderate injury by heavy weight of the instrument.

• Consult a second person to transport the instrument

• Do not drop the instrument

• Place the instrument on a stable, even and vibration-free surface

• Keep limbs out of crushing zone

34 B-90 Operation Manual, Version B

5.2 Installing the Nano Spray Dryer B-90



Switch off the instrument and remove the power cord before any work described in section 5.

5.2.1 Tall set-up with long metal bars

NOTE

Parts (a – e) and the black holders (i), are factory pre-installed.



5 Putting into operation



a Screw the four lower metal bars into the housing basement with a ﬂat spanner. b Fix the four adjusting rings onto the previously installed metal bars. c Mount four short headless screws onto the lower metal bars. Use a hex-wrench to screw them

tightly in.

d Screw the middle metal bars tightly onto the lower ones. e Mount four short headless screws onto the middle metal bars. Use a hex-wrench to screw them

tightly in.

f Screw the four upper metal bars onto the middle ones and screw them tightly together. g Mount the four long headless screws onto the upper metal bars. Use a hex-wrench to screw

them tightly in.

h Put the four counter nuts upside-down and onto the long headless screws on top of the bars and

turn them clockwise to the lowest possible position.

i To install the bar holders, ﬁrst screw the holder base at the housing. Use the metal bars for align-

ment. Subsequently attach the side of the holders with the side caps and three screws.

35 B-90 Operation Manual, Version B

5.2.2 Short set-up with short metal bars

NOTE

Parts (a – e) and the black holders (g), are factory pre-installed.







5 Putting into operation









them tightly in.

d Screw the middle metal bars tightly onto the lower ones. e Mount the four long headless screws onto the upper metal bars. Use a hex-wrench to screw

them tightly in.

f Put the four counter nuts upside-down and onto the long headless screws on top of the bars and

turn them clockwise to the lowest possible position.

g To install the bar holders, ﬁrst screw the holder base at the housing. Use the metal bars for align-

ment. Subsequently attach the side of the holders with the side caps and three screws.

36 B-90 Operation Manual, Version B

5.3 Sub-assembly installations

Switch off the instrument and remove the power cord before any installation work.

5.3.1 Lifting device

5 Putting into operation

a Position the lifting device, using the three bottom

sided timing holes, onto the matching knobs at the instrument’s basement.

b Rotate the lifting device some degrees clockwise to

ﬁx it tightly by hand. The lever has to be positioned towards the front.

70 mm

c Screw the gas outlet part onto the lifting device with

two hex-wrench screws.

d Take the small o-ring from the set of sealings (order

no. 051775). Place it on the sealing seat of the gas outlet part.

e Install the outlet temperature sensor at the gas

outlet part. For the correct installation depth keep the sensor housing approximately 70 mm out of the gas outlet part. Use a ﬂat spanner to ﬁx the screw ﬁtting of the sensor housing tightly

Subsequently connect the outlet temperature sensor plug to socket (see section 4.10, socket b).

37 B-90 Operation Manual, Version B

5.3.2 Electrode assembly installation

Caution

Risk of minor or moderate injury by electric shock.

• Switch off the instrument before connecting or disconnecting the high-voltage cable

• Do not touch the high-voltage cable with wet hands

• Use only damage free cabling

NOTE

Before installing the electrode, clean all parts a to e thoroughly.

5 Putting into operation

a Position the ﬂat seal at the particle collector

basement.

b Position the metal collecting tube electrode

on the collector basement and assure electrical contact. The broader uncoated stripe at the lower outer side is to be installed towards the base.

c Install the insulation glass cylinder on the

collector basement.

d Place the assembly on the lifting device.









38 B-90 Operation Manual, Version B



5 Putting into operation

e Use the protective grid holder to carefully

insert the HV-electrode into its seat at the bottom plate of the particle collector. Clean and dry this part before installation.



f To unlock the protective grid, open the

spring lock at the handling knob ﬁrst. Carefully lift off the grid from the HVelectrode in a vertical upwards movement.

Finally, connect the electrical cable of the particle collector to the high voltage socket at the frontside of the instrument (see section

4.10, socket a) and ﬁx it hand-tight.

39 B-90 Operation Manual, Version B

5 Putting into operation



5.3.3 Glass cylinder installation

Risk of minor or moderate cuts when handling damaged glass parts.

• Handle glass parts with care

• Visually inspect every glass part before mounting

• Exchange damaged glass parts immediately

• Do not touch cracks or bits of broken glass with bare hands



Caution

g Put the plastic distance sheet on top of the

electrode cylinder.

h Put the centerpiece holder on the plastic

distance sheet.

i Adjust the four screw rings on the metal

bars to touch the underside of the distance sheet. Fix them tightly with an hex-wrench.

Finally, remove the plastic distance sheet again by pulling it out towards the front.

After correct installation it is possible to remove the complete electrode cylinder assembly towards the front.

NOTE

Clean all glass parts before mounting to avoid cross contamination.

Cylinder assembly tall set-up

a Mount a ﬂat sealing ring on the bottom of the lower

glass cylinder.

b Place the glass cylinder on the centerpiece holder.



c Position the glass-to-glass sealing on top of the

lower glass cylinder. The smaller diameter has to be on top towards the spray cylinder.

d Position the second ﬂat sealing ring on top of the

spray cylinder.

e Place the spray cylinder on top of the glass-to-glass

sealing.

All sealings are part of the sealing set (order no. 051778).

40 B-90 Operation Manual, Version B





Cylinder assembly short set-up



5 Putting into operation

a Mount a ﬂat sealing ring on the bottom of the spray

cylinder.

b Position the second ﬂat sealing ring on the spray

cylinder.

c Place the spray cylinder on the centerpiece holder.

All sealings are part of the sealing set (order no. 051778).

5.3.4 Heater module installation



Special mounting tool in position.

Caution

Risk of minor or moderate burning when handling hot parts.

• Do not touch hot parts

• Let the system cool down for some minutes after use

The special mounting tool serves as a mounting gauge for the correct distance of all mounted parts between

lifting device and heater.

• Put the lever arm of the lifting device into the end a of the tool ﬁrst. The tool and the handle are equipped with holes. Line up all holes and insert a hex-wrench through the holes to stabilize the correct tool position.

• Use the left metal bar to support the tool end b.

The lifting device is now in mounting height for the heater module installation.

41 B-90 Operation Manual, Version B

5 Putting into operation

c Mount the inlet temperature sensor at the heater

module. Keep the temperature sensor end about



70 mm out of the screw connection. Use a ﬂat spanner to tighten the screw ﬁtting.

d Place the heater module on the metal screw bars.

NOTE

• Position four hex nuts from top onto the metal bar ends with a narrow gap towards the heater module.

• Position the hex nuts from below the heater with approximately the same narrow gap towards the heater module.

All nuts must be tightened crosswise only!





Make sure the spray cylinder is in-line with the heater module and that the sealing is properly placed between. e–f Tighten the hex counter nuts above and below

the heater crosswise. Do not overtighten the nuts.

g Remove the mounting tool from the lifting device

after installation.

Final steps:

• Connect the electrical cable of the heater to the

back side of the instrument (see section 4.10, socket m).

• Connect the inlet temperature sensor to its socket

at the back side of the instrument (see section 4.10, socket l).

• Connect the drying gas tubing to the inlet of the

heater module. Use a hose clamp for ﬁxation.

• Connect the drying gas tubing between the heater

inlet and the connector nipple inside the instrument (open the upper back panel of the instrument to get access).

42 B-90 Operation Manual, Version B

5.4 Spray head assembling and installation

The spray head is a major part of the whole spray drying process. To ensure proper function and highest yield, dry and clean conditions of all parts during assembling and installation are required. For detailed cleaning information see section 8.6.1.

Caution

Risk of minor or moderate burning when handling hot parts.

• Do not touch hot parts

• Let the system cool down for some minutes after use

5.4.1 Spray head assembling

5 Putting into operation

a Spray head

b Screw M3; torx

f g h i

c Rubber sealing

d Head holder

e Seal for electrical cable

f Fitting

g Silicone seal (o-ring)

h Ferrules

i Tube connector

43 B-90 Operation Manual, Version B

5 Putting into operation

j Feed tubing

k Spray cap

NOTE

• Only use original BUCHI parts for installation.

• Small parts (e–j) are available in the set „Set of feed tubing connections complete“ with

order no. 051768.

Assembly steps

1. Put the “Silicone seal” g onto the two “Fittings” f and screw them into the head holder hand-tight.

2. Introduce the “Rubber sealing” c onto the head holder.

3. Mount the spray head at the “Head holder” d. See also section 5.3.2 for details.

4. Insert the electrical cable through the cable hole of the “Head holder”.

44 B-90 Operation Manual, Version B

5 Putting into operation

5. Introduce the “Seal for electrical cable” e and tighten the cable bushing using a ﬂat spanner.

6. Introduce the “Feed tubing” j through the spray head.

7. Screw the “Spray cap” k onto the spray head.

8. Introduce the “Feed tubing” k into the “Fittings” f. Attach the “Ferrules” h to the “Feed tubing”.

9. Mout the “Tube connectors” i at the “Fittings”.

45 B-90 Operation Manual, Version B

5 Putting into operation



NOTE

Tighten the spray cap and washer assembly with a torque of 7 Nm.

10. Use the mounting tool a and the BUCHI torque wrench b for the installation of the spray cap.

Installation steps:

11. Use the thumb screw and ﬁxate the mounting tool at one of the lower metal bars of the Nano Spray Dryer B-90.

12. Mount the spray cap on the spray head hand-tight.

13. Put the spray head through the hole of the mounting tool.

14. Use the BUCHI torque wrench to fasten the spray cap at the spray head with a torque of 7 Nm.

15. Remove the spray head with the mounted spray cap from the mounting tool.

16. Remove the mounting tool from the metal bar.

17. Install the spray head on the spray cylinder.

18. Align the “Tube connectors” i and the electrical cable connection vertically, so that the head is spraying downwards.

19. Mount the spray head in the shown order (A to B) and in the direction of the arrow.

20. Connect the spray head cable to the socket labelled with “SPRAY” at the housing front.

46 B-90 Operation Manual, Version B

5.4.2 Spray head installation

The spray head can be mounted at the spray head holder in either an angular or horizontal position. The most appropriate position depends on the sample product and its spray drying requirements. In all three angular positions the thermal load of the spray head is considerably decreased because the spray head is out of the central ﬂow of the hot drying gas. This makes the angular position an option for spraying heat-sensitive materials.



30°

5 Putting into operation

For angular spray head position:

• To set the angulation of the spray head holder remove the angulation screw a ﬁrst. Then swivel the spray head holder to the desired angle (30°, 45° or 60°) and reattach the screw in the chosen angle. Fasten the screw again.

• To mount the spray head, use a small torx screw (M3×16) to ﬁx it at the holder b.

45°

30°

60°



For vertical spray head position:

To mount the spray head in vertical position c, use a small torx screw to ﬁx it at the holder.

5.5 Peristaltic pump and feed tubing installation

The peristaltic pump uses a pulley drive to transport liquids through the tubing. The pump design is dry run safe. During the spray drying process it constantly feeds the spray head with sample liquid.

Risk of instrument short-circuits and damage by liquids.

• Do not spill liquids over the instrument or parts of it

• Wipe off any liquids instantly

• Place the sample vessel onto the designated reservoir-plate on top of the instrument

• Ensure a safe positioning of the sample vessel

• Do not move the instrument when it is loaded with liquid

• Keep external vibrations away from the instrument

Notice

47 B-90 Operation Manual, Version B

5.5.1 Peristaltic pump height adjustment and ﬁxation

5 Putting into operation

a Mount the peristaltic pump on a metal bar and ﬁx it with the thumb screw. b To adjust the height, unfasten the thumb screw and move the pump to the optimal height. Fasten

the thumb screw again to ﬁxate the pumps position.

c Connect the power cable of the pump to the socket labelled with “PUMP” at the housing front.

5.5.2 Pump bed adjustment

a Turn the lever horizontally to the left. Pre-adjust the pump bed to working position for liquid

transport with a hex-wrench. The correct position depends on the thickness of the transport tube material.

b Place the tube in the pump mechanism. Swivel the lever towards the locking of the pump bed.

The pump is set up correctly when the tube is squeezed between the pulleys without damaging the tube.

48 B-90 Operation Manual, Version B

5.5.3 Feeding tube installation

Steps before installation:

• Switch off the Nano Spray Dryer B-90.

• Place the sample vessel on the top cover of the instrument or on the stand plate.

• Choose the silicone tubing for aqueous applications or alternatively the appropriate tygon type for other solvents (see also Table 5-1 for a list of most common solvents).

5 Putting into operation

Sample vessel

a Install the feeding tube at the peristaltic pump ﬁrst. Make sure the plastic manifold is seated in the

right holder of the pump mechanism (see example photo below). Connect the tube to the spray head. The inlet and outlet positions depend on the internal tubing of the spray head. Place the free end of the tube in the sample vessel.

b Connect a second tube at the spray head and place its free end in the sample vessel.

49 B-90 Operation Manual, Version B

5 Putting into operation

Example photo with attached feeding tube and adapter piece (transparent adapter on the pump inlet at the right side).

Table 5-1: Choosing the feeding tube material

Solvent Silicone tube Tygon MH 2075 Tygon F 4040 A

Methanol suitable suitable suitable

Ethanol suitable suitable suitable

Acetone unsuitable suitable unsuitable

Toluene unsuitable unsuitable suitable

Isopropanol suitable suitable suitable

Chloroform unsuitable unsuitable unsuitable

Dichloromethane unsuitable unsuitable unsuitable

THF unsuitable unsuitable unsuitable

Ethylacetate unsuitable suitable unsuitable

Hexane unsuitable unsuitable suitable

Water suitable suitable suitable

50 B-90 Operation Manual, Version B

5.6 Drying gas supply

The kind of drying gas supply (air or inert gases) depends on the kind of processed sample material. There are signiﬁcant differences between ‘open loop’ and ‘closed loop’ conﬁguration of supply and exhaust gases. Strictly follow the conﬁguration descriptions in this section as well as the deﬁned proper and improper use in section 2 for safe operation.

Death by suffocation or serious poisoning by inhalation of inert gases.

• Do not inhale inert gases

• Directly withdraw released gases and gaseous substances by sufﬁcient ventilation

• Only operate the instrument in ventilated environments

• Before operation, check all parts, connections and sealings involved in the gasﬂow for proper

• Exchange worn out or defective parts immediately

sealing

5 Putting into operation

Danger

Warning

Death or serious poisoning by contact or incorporation of harmful substances at use.

• Before operation, check the instrument for correct assembling

• Before operation, inspect sealings and tubes for good condition

• Exchange worn out or defective parts immediately

• Exchange clogged ﬁlters immediately

• Only operate the instrument in ventilated environments

• Directly withdraw released gases and gaseous substances by sufﬁcient ventilation

• Perform a dry-run without sample material and check for gas leakages

Warning

Death or serious injuries by compressed gas.

• Depressurize gas circuit before any modiﬁcation

• Wear safety goggles

Risk of instrument damage by wrong gas supply.

• All labels at gas connections must be clearly ledgible

• Before operation, check all gas connections for correct installation

• External supply pressure must meet the system speciﬁcations

51 B-90 Operation Manual, Version B

Notice

5.6.1 ‘open loop’ air supply conﬁguration

In ‘open loop’, compressed air or the Aspirator in blowing mode with inlet ﬁlter is required to establish the necessary drying gas overpressure. To ensure the optimal drying air performance in this operation mode, the supplied air has to be dry and free of impurities. If this can not be guaranteed, BUCHI recommends the use of a Wilkerson air maintenance unit (see next picture).

When working with pressurized gases:

• Turn off the pressure source and remove the power cord before installation work.

• Depressurize all system parts and supply tubes.

NOTE

If there is no compressed air available, the compressed air can also be supplied by an oil-free compressor.

5 Putting into operation

a Coarse ﬁlter b Submicron ﬁlter c Activated charcoal ﬁlter

The optional Wilkerson air unit is to be installed between a compressed air source and the Nano Spray Dryer B-90 air inlet. For installation, see documentation of the Wilkerson air maintenance unit!

The drying air connection is located on the right side of the instrument (see section 4.10 for details). The connections are made via Polypress and Solaﬂex tubing in combination with clamp ﬁttings. Any exhaust gases must be safely withdrawn (e.g. through a fume hood).

a GAS OUT (Polypress with clamp ﬁtting) b GAS IN (Polypress/Solaﬂex with clamp ﬁtting) c Flow regulation valve (only necessary with direct

compressed air supply)

52 B-90 Operation Manual, Version B

5.6.2 ‘closed loop’ gas supply conﬁguration

The Nano Spray Dryer B-90 Advanced has been designed to be used in ‘closed loop’. This mode is universal and can be used to spray dry aqueous as well as solvent mixtures with air or inert gas under safe conditions. To ensure the optimal drying gas performance in this operation mode the supplied gas has to be dry and free of impurities.

5 Putting into operation

The drying gas connections are located on the right side of the instrument (see section 4.10 for details). The connections are made via Polypress and Solaﬂex tubing in combination with clamp ﬁttings and via quick coupling connection. The kind of connection depends on the type socket and the transported gases. The output gas is recycled by an Inert Loop B-295/Dehumidiﬁer B-296. In ‘closed loop’ mode, the Aspirator works as a recirculating pump to establish a constant gas ﬂow.

5.6.3 Outlet ﬁlter installation/replacement

The Nano Spray Dryer B-90 is equipped with a safety outlet ﬁlter. This particle ﬁlter (order no. 051656) has an efﬁciency of 99.9 % for particles < 1 µm. The ﬁlter should be replaced when clogged. This is

indicated by a strong pressure drop (see also the error messages in chapter 8.1). Switch off the instrument, remove the power cord before installation work and depressurize the system and all supply

tubes.

Danger

Death or serious poisoning by gases or particles at O2– sensor or ﬁlter malfunction

• Exchange defective O2– sensor immediately

• Exchange O2– sensor regularly within the speciﬁed maintenance intervals

• Exchange clogged ﬁlters immediately

• Exchange ﬁlters regularly within the speciﬁed maintenance intervals

• Safely dispose ﬁlter immediately

a GAS OUT (Polypress with clamp ﬁtting) b N2 (quick coupling) c AIR (CO2) (quick coupling) d GAS IN (Polypress with clamp ﬁtting)

Risk of instrument damage by internal overpressure.

• External supply pressure must meet the system speciﬁcations

• Exchange clogged ﬁlters immediately

• Safely dispose ﬁlter immediately

53 B-90 Operation Manual, Version B

Notice

5 Putting into operation

• Disconnect the power cord from the mains.

• Gently pull off the back panel of the housing and put it aside. The outlet ﬁlter is now directly accessible.

• Loosen the hose clamps to remove the ﬁlter element.

• Put in the new ﬁlter and fasten the hose clamps again.

• Connect the power cord to the mains. The device

can now be switched on.

NOTE

The ﬁlter has a designated gas ﬂow direction. To ensure maximum throughput and ﬁlter lifetime it should be installed correctly. The designated ﬂow direction is indicated by an arrow on the ﬁlter housing. For correct alignment, the arrow has to point towards the gas outlet connector of the Nano Spray Dryer B-90 when installing the ﬁlter. After exchange, dispose used ﬁlter according to local regulations immediately.

5.7 Aspirator installation modes

To establish the required instrument input pressure for the drying medium ﬂow, the output of the Aspirator can be used in blowing mode. The Aspirator can be part of an ‘open loop’ conﬁguration. In ‘closed loop’ the use of an Aspirator is required.

5.7.1 Aspirator in ‘open loop’ conﬁguration

Installation steps

1. Disconnect the power cord from the mains and depressurize all system parts.

2. Connect the air inlet ﬁlter (011235) to the aspirators air inlet a

3. Connect the air outlet b to the Nano Spray Dryer B-90 gas inlet.

4. Connect the power cord to the mains. The device can now be switched on.

a Air inlet with ﬁlter b Air outlet towards gas inlet connector of the Nano

Spray Dryer B-90 in Polypress design

c Output ﬂow-through selector (frequency based

regulation)

d Mains socket, switch and fuse box

The Aspirator has a bench top dimension of 47,5×30×32 cm and can be placed beside the Nano Spray Dryer B-90 or on the tray of the trolley.

NOTE

The Aspirator can not be used in combination with the ﬂow regulation valve. Remove the ﬂow regula-

tion valve if mounted.

54 B-90 Operation Manual, Version B

5.7.2 Aspirator in ‘closed loop’ conﬁguration

This operation mode is only available in combination with a Nano Spray Dryer B-90 Advanced model.

5 Putting into operation

a Gas inlet (connection to outlet of Inert Loop B-295

or Dehumidiﬁer B-296)

b Gas outlet towards gas inlet connector of the Nano

Spray Dryer B-90 in Polypress design

c Output ﬂow-through selector (frequency based

regulation)

d Mains socket, switch and fuse box

The Aspirator has a bench top dimension of 47,5×30×32 cm and can be placed beside the Nano Spray Dryer B-90 Advanced or on the tray of the trolley.

Installation steps

1. Disconnect the power cord from the mains and depressurize all system parts.

2. Connect the gas inlet a to the outlet of Inert Loop B-295 or Dehumidiﬁer B-296.

3. Connect the gas outlet b to the GAS IN connection of Nano Spray Dryer B-90 Advanced.

4. Connect the power cord to the mains. The device can now be switched on.

NOTE

The Aspirator can not be used in combination with the ﬂow regulation valve. Remove the ﬂow regula-

tion valve if mounted.

5.8 Inert Loop B-295 installation

In ‘closed loop’ the Nano Spray Dryer B-90 Advanced can be combined with the Inert Loop B-295 upgrade set and the Aspirator. This enables spray drying of organic solvent solutions under inert conditions in a fume hood or equivalent. Additionally an adsorption column can be installed to dry the recirculating gas.

Danger

Death by suffocation or serious poisoning by inhalation of inert gases.

• Do not inhale inert gases

• Directly withdraw released gases and gaseous substances by sufﬁcient ventilation

• Only operate the instrument in ventilated environments

• Before operation, check all parts, connections and sealings involved in the gasﬂow for proper sealing

• Exchange worn out or defective parts immediately

55 B-90 Operation Manual, Version B

5 Putting into operation

Danger

Death or serious poisoning by gases or particles at O2– sensor or ﬁlter malfunction

• Exchange defective O2– sensor immediately

• Exchange O2– sensor regularly within the speciﬁed maintenance intervals

• Exchange clogged ﬁlters immediately

• Exchange ﬁlters regularly within the speciﬁed maintenance intervals

• Safely dispose ﬁlter immediately

Warning

Death or serious injuries by compressed gas.

• Depressurize gas circuit before any modiﬁcation work

• Wear safety goggles

Warning

Death or serious poisoning by contact or incorporation of condensed liquid.

• Dispose of condensate safely after use

• Wear safety gloves

Risk of instrument damage by wrong gas supply.

• All labels at gas connections must be clearly ledgible

• Before operation, check all gas connections for correct installation

• External supply pressure must meet the system speciﬁcations

Risk of instrument damage by internal overpressure.

• External supply pressure must meet the system speciﬁcations

• Exchange clogged ﬁlters immediately

• Safely dispose ﬁlter immediately

Notice

56 B-90 Operation Manual, Version B

5.8.1 Main device installation

During the process, a constant inert gas ﬂow (N2 or CO2) is fed into the gas loop to refresh the used drying gas. This constant gas feeding requires an exhaust gas output to balance the pressure inside the gas circuit, thereforee the Inert Loop B-295 is equiped with a hose connection for the exhaust gas at its right side. The use of inert gas requires additional safety measures. The upgrade set for the Inert Loop B-295 (order no. 051783) is required to work in ‘closed loop’ operation with Nano Spray Dryer B-90 Advanced. The set includes a back pressure check valve, hose connectors and compressed gas tubing for CO2 and N2.

5 Putting into operation

a Communication cable to the Nano Spray Dryer B-90

Advanced (see section 4.10; socket c)

b Oxygen concentration display window c Solvent condensate collector

The Inert Loop B-295 has transport wheels mounted and can be placed next to a fume hood, near the Nano Spray Dryer B-90 Advanced in the lab.

The communication cable a is part of the oxygen safety loop. When the oxygen content reaches 6 % the spray drying will be interrupted and an error message will be displayed at the Nano Spray Dryer B-90 Advanced.

d Gas outlet towards gas inlet of the Aspirator (see

section 5.5.2)

e Gas inlet connected to the gas outlet of the Nano

Spray Dryer B-90 Advanced

f Exhaust gas outlet towards check valve g

g Check valve with exhaust gas tube

(to connection f )

57 B-90 Operation Manual, Version B

Installation steps

1. Disconnect the power cord from the mains and depressurize all system parts.

2. Install the check valve at the exhaust gas tubing outlet and lead it to a fume hood or ventilation system.

3. Connect all tubes (see pictures).

4. Connect the communication cable to the Nano Spray Dryer B-90 Advanced.

5. Connect the power cord to the mains. The device can now be switched on.

NOTE

If air is sucked in through the tube during operation, this is an indication that the ‘closed loop’ is not tight. Switch off the assembly and re-check all connections and sealings immediately. Take out the necessary corrective actions to obtain a sealed conﬁguration.

5.9 Dehumidiﬁer B-296 installation

The Dehumidiﬁer B-296 can be used for reproducible inlet air conditioning by condensation of water/ solvent residues in gases. It works at a ﬁxed cooling temperature of 0 °C.

5 Putting into operation

Warning

Death or serious poisoning by contact or incorporation of condensed liquid.

• Dispose of condensate safely after use

• Wear safety gloves

58 B-90 Operation Manual, Version B

5.9.1 Dehumidiﬁer B-296 in ‘open loop’ conﬁguration

When aqueous sample materials are being processed in open-mode and with the Aspirator with inlet ﬁlter as an air supply source, the use of the Dehumidiﬁer B-296 is highly recommended.

5 Putting into operation

a Input/Output gas connectors (Polypress style)

b System status display

c Power switch

d Attached condensate vessel

Installation steps

1. Disconnect the power cord from the mains and depressurize all system parts.

2. Place the Dehumidiﬁer B-296 next to the Nano Spray Dryer B-90 and the Aspirator.

3. Connect the tubing from the outlet (labelled on the enclosure) of the Dehumidiﬁer B-296 to the gas inlet of the Nano Spray Dryer B-90 (see section 4.10; connector h). Use hose clamps to ﬁx the tubing.

4. Connect the tubing from the Aspirator outlet (see section 5.6.1; connector b) to the inlet of the Dehumidiﬁer B-296 (labelled on the enclosure). Use hose clamps to ﬁx the tubing.

5. Connect the inlet ﬁlter to the gas inlet of the Aspirator. Use a hose clamp to ﬁx the tubing.

6. Connect the power cord to the mains. The device can now be switched on.

59 B-90 Operation Manual, Version B

5.9.2 Dehumidiﬁer B-296 in ‘closed loop’ conﬁguration with out Inert Loop B-295

When mixtures of organic solvents and water (with less than 50 % solvents) are being processed in ‘closed loop’ conﬁguration, the use of the Dehumidiﬁer B-296 in combination with a heat exchanger is highly recommended. The optional heat exchanger increases the condensation performance and can additionally reduce the residual solvent/water content of the spray dried material.

a Inlet tubing B-296 b Outlet tubing B-296

5 Putting into operation

Installation steps

1. Disconnect the power cord from the mains and depressurize all system parts.

2. Place the Dehumidiﬁer B-296 next to the Nano Spray Dryer B-90 and the Aspirator.

3. Connect the tubing b from the outlet (labelled on the enclosure) of the Dehumidiﬁer B-296 to the

gas inlet of the Aspirator (see section 5.6.1; connector a). An additional tube is needed.

4. Connect the Aspirator outlet to the inlet of the Nano Spray Dryer B-90 (see section 4.10,

connector h).

5. Connect the tubing from the Nano Spray Dryer B-90 outlet (see section 5.6.1; connector b) to

the inlet a of the Dehumidiﬁer B-296 (labelled on the enclosure). An additional tube is needed.

6. Use hose clamps to ﬁx all Polypress tubings.

7. Connect the power cord to the mains. The device can now be switched on.

5.9.3 Adsorption column installation

If mixtures of organic solvents and water are used, the Dehumidiﬁer B-296 is strongly recommended for a ‘closed loop’ conﬁguration. The Dehumidiﬁer B-296 removes the water from the drying gas before entering the Inert Loop B-295. This separation prevents water from freezing in the Inert Loop B-295 and potential damage of the heat exchanger.

NOTE

The upgrade kit for the Inert Loop B-295 has to be installed according to the chapter 5.8.1

60 B-90 Operation Manual, Version B

5 Putting into operation

a Outlet of the Nano Spray Dryer B-90 c Outlet of the Inert Loop B-295 b Outlet of the Dehumidiﬁer B-296

Installation steps

1. Disconnect the power cord from the mains and depressurize all system parts.

2. Put the holder of the adsorption column e on the Inert Loop B-295 and ﬁx it with the adhesive tape.

3. Attach the adsorption column with the installed sieve bag and the humidity sensor a at the holder e.

4. Connect the inlet tube d of the adsorption column to “GAS OUT” at the Nano Spray Dryer Advanced B-90 (see section 4.10; connector e). Use hose clamps to ﬁx the tubing.

5. Connect the adsorption unit outlet tube c from the column outlet at the humidity sensor to the Inert Loop B-295 inlet. Use hose clamps to ﬁx the tubing.

6. Connect the outlet of the Inert Loop B-295 to the inlet of the Aspirator (see section 5.6.1; gas inlet a). Use hose clamps to ﬁx the tubing.

7. Connect the gas outlet of the Aspirator to the GAS IN at the Nano Spray Dryer Advanced B-90. Use hose clamps to ﬁx the tubing.

8. Plug in the Inert Loop B-295 communication cable (see section 5.7; cable a) into the external electronic box b. Secure the electronic box with double-faced adhesive tape at the housing.

9. Plug the humidity sensor cable into the external electronic box b.

10. Plug the communication cable of the electronic box into the Nano Spray Dryer B-90 (see section

4.10; socket c).

11. Connect cooling water or a recirculating water chiller to the double jacket of the adsorption column (see section 5.7.2; connectors f) if passive cooling is not sufﬁcient.

12. Connect the inlet ﬁlter to the gas inlet of the Aspirator. Use a hose clamp to ﬁx the tubing.

13. Connect the power cord to the mains. The device can now be switched on.

61 B-90 Operation Manual, Version B

5.10 Final installation check

This check has to be carried out after every installation and prior to the ﬁrst spray drying process. All connected supply media (e.g. mains voltage and gas pressure) must match the technical data of the installed system or system set-up.

• Inspect all glass components for damage.

• Check the gas tubing connections and gas supply for leakages and good condition.

• Check that the complete set-up is sealed tightly and in sequence.

• Switch off the Nano Spray Dryer B-90. Check the high voltage cable of the electrical particle

collector for proper seating.

• Check all other electrical connections for proper connection, such as optional or external compo-

nents, for example: temperature sensors, heater, peristaltic pump cabling. The number of sensors to be checked depends on the actual conﬁguration.

NOTE

At 100 liter/minute gas ﬂow, the internal pressure reading should be in the range of 30 to 60 mbar for a well sealed system in ‘open loop’.

5 Putting into operation

5.11 Electrical connections

After the installation procedure and the ﬁnal check has been completed successfully, the power plug of the Nano Spray Dryer B-90 and optional instruments must be connected to the mains for the spray drying process.

Risk of instrument damage by wrong mains supply.

• External mains supply must meet the voltage given on the type plate

• Check for sufﬁcient grounding

The used mains circuit has to:

• provide the voltage that is given on the type plate of the instrument.

• be able to handle the load of the connected instruments.

• be equipped with adequat fusage and electrical safety measures, in particular proper earthing.

See also technical data of all components regarding the different minimum system requirements!

Notice

NOTE

Additional electrical safety measures such as residual current brakers may be necessary to meet local laws and regulations! External connections and extension lines must be provided with an earthed conductor lead (3-pole couplings, cord or plug equipment). All used power cords shall be equipped with molded plugs only to avoid risks due to unobservant defective wiring.

62 B-90 Operation Manual, Version B

6 Operation

This chapter gives examples of typical instrument applications and instructions on how to operate the instrument properly and safely. See also section 2.5 “Product safety” for general warnings.

6.1 Starting up the instrument

• Make sure the Nano Spray Dryer B-90 is properly connected to the mains supply.

• Carry out a ﬁnal installation check (see section 5.9) before every spray drying process.

• Switch on the Nano Spray Dryer B-90 at the main switch.

• Switch on all other electrical devices of the actual conﬁguration at their main switch.

6.2 Main screen

After the internal system check at bootup ﬁnished successfully, the main screen view below appears at the Nano Spray Dryer B-90.

6 Operation

a Display showing the current instrument status b Pump button to adjust the pump rate c Spray button to change the relative spray rate d Temp button to change the inlet temperature e Menu button to enter the ﬁrmware menu structure

c d e

f Heat button to switch the heater ON/OFF g Spray button to switch spray function ON/OFF h Pump button to switch the pump ON/OFF i Selection knob to change process parameters and

instrument conﬁguration

(Peristaltic) Pump selection Four digits (1–4) are selectable:

1 — Clockwise pump rotation at standard speed 2 — Clockwise pump rotation at double speed

63 B-90 Operation Manual, Version B

3 — Pump rotation direction alternates every 3 seconds 4 — Pump rotation direction alternates every 6 seconds

Spray selection Select a spray head output between 0 % and 100 % spray rate. This directly effects the throughput of

the spray head.

Temperature selection Set the drying gas inlet temperature between 0 °C to 120 °C.

NOTE

The lowest possible drying gas inlet temperature in ‘open loop’ mode depends on the local room temperature.

6.3 Menu structure overview

The table below shows all Nano Spray Dryer B-90 menus available from “Standard view” to “Sub– Menu 3”.

6 Operation

Basic state

Standard view

Pump

Spray

Temp.

Sub–Menu 1

View Parameters

Gas Mode

Conﬁguration

Air ~4 % O ~1 % O

Sub–Menu 2 Sub–Menu 3

Units

LCD-Contrast

Sea Level

Rot Release

Key Sound

Temperature

Volumeﬂow

Pressure

Calibration

Language

Info

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6.4 Display elements and menu functions

6.4.1 Operating controls

Multifunctional buttons The multifunctional buttons below the screen are programmable. Their actual use is displayed on the

screen directly above the buttons.

a b c d

6 Operation

a Go back one step/Escape b Move cursor upwards c Move cursor downwards d Enter next menu level/OK (conﬁrm selection)

Rotary knob The rotary knob is used to select values out of lists within sub menus.

• Turning the knob clockwise moves the cursor downwards

• Turning the knob anticlockwise moves the cursor upwards

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6.4.2 View parameters menu

To enter the “Menu” press the corresponding multifunctional button below the screen. Inside the menu, use the multifunctional buttons for navigation.

The “View parameters” menu and its sub menus provide information about the actual system status. It is accessible at any time and can supply the user with useful information about ongoing processes. No changes can be made here.

6 Operation

NOTE

In ‘closed loop’ mode the N2 and O2 valve open and close depending on the O2 content in the gas loop to maintain the selected O2 concentration (< 4 % or <1 %).

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6.4.3 Gas mode selection menu

To enter the “Menu” press the corresponding multifunctional button below the screen. Inside the menu, use the multifunctional buttons for navigation.

Select “Gas mode” and enter the selection. Select the correct setting for the actual spray drying process and conﬁrm the selection with “OK”.

6 Operation

NOTE

• Set to “Air” for ‘open loop’ mode

• Set to “~4 % O2” for ‘closed loop’ mode with inert gas N2 and CO2 (only Nano Spray Dryer B-90

Advanced)

• Set to “~1 % O2” for ‘closed loop’ mode with increased inert gas N2 and CO2 consumption (for

oxygen and ozone sensitive material; only Nano Spray Dryer B-90 Advanced)

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6.4.4 Conﬁguration menu

To enter the “Menu” press the corresponding multifunctional button below the screen. Inside the menu, use the multifunctional buttons for navigation to “Conﬁguration” and conﬁrm the selection.

6 Operation

Items in menu “Conﬁguration”: Description / available parameters:

Units

LCD-Contrast

Sea level

Rot. release

Key sound

Language

• Temperature in °C, K or °F

• Volume ﬂow in l/min, m3/h, ft3/h

• Pressure in mbar, Torr, hPa

Select a screen contrast between 0 and 100 %.

Select the sea level in meters over sea level.

Deﬁnes the time interval in which the rotary knob is active after pressing the selection buttons for “Pump”, “Spray” and “Temp.”. The default time is 3 seconds. This is a feature to avoid unintended inputs.

If “YES” is selected a sound is audible when pressing a function key. To suppress the acoustic conﬁrmation select “NO”.

Choose the language of the user interface between Chinese, English, French, German, Italian, Japanese or Spanish.

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6.4.5 Firmware calibration menu

To enter the “Menu” press the corresponding multifunctional button below the screen. Inside the menu, use the multifunctional buttons for navigation to “Calibration”. Stop the gas ﬂow and conﬁrm by pressing the “OK” button to recalibrate the internal ﬂow sensor of the Nano Spray Dryer B-90.

6 Operation

NOTE

The calibration should be performed periodically to ensure best spray drying results.

6.4.6 Firmware info menu

This menu displays the current system software version in eight digits. It appears after every boot up for an instant and can be reviewed via the “Info” menu entry. The ﬁrmware version can be useful during service.

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6.5 Starting a spray drying process

System preconditions All system items must be correctly installed according to the kind of set-up, see section 5 for more

information. Carry out a ﬁnal installation check (see section 5.9) before every spray drying process. See also section 2.5 “Product safety” for general warnings.

Danger

Death or serious poisoning by inhalation or incorporation of dried particles during spray process.

• Wear safety goggles

• Wear safety gloves

• Wear a suitable protective mask

• Wear a laboratory coat

• Check for proper sealing before use

• Do not inhale dried particles

• Stop drying gas ﬂow before opening the drying circuit

6 Operation

Starting a spray drying process

1. Switch on the instrument. After the automatic self check, the operating mode is activated.

2. Switch on all other devices if installed in the current conﬁguration.

3. Set the drying gas rate to a reasonable ﬂow of about 70–150 liter/min with the external gas regulator (when using compressed gas) or adjust the frequency controller when using the Aspirator (set a rotational frequency between 30–40 Hz).

4. Read the relative inside pressure (typical pressure range 30 mbar to 60 mbar).

5. Select the desired inlet temperature (typical setting between 80 °C to 120 °C).

6. Switch on the heater by pressing the “Heat” button and wait until the system has reached stationary temperature conditions (typically after 5 to 10 min.).

7. Switch on the peristaltic pump by pressing the “Pump” button.

8. Select the relative spray rate (typically 100 % to achieve maximum throughput).

9. Press the “Spray” button to start the spray process.

The spray process starts and the electrical ﬁeld in the particle collector is turned on.

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6.6 Optimizing parameters

The relevant parameters for the spray drying process depend on each other.

List of spray drying parameters

• drying gas ﬂow rate

• relative inside pressure

• inlet temperature

• feed rate

The properties of the spray dried solution determines the maximum process temperature. The maximum thermal load of the solid particles is caused by the spray head temperature or by the maximum inlet drying gas temperature. To reduce the thermal load on the feed, the sample vessel maybe cooled.

The achievable droplet sizes depend on the installed spray cap. Mean values for water applications are shown in the following table.

6 Operation

Table 6-1: Spray nuts

Spray cap

(hole size)

Mean water

droplet size (D

Approx. water

)

throughput

4,3

Span

D90 - D

( )

4.0 µm 8 µm 10 – 20 mL/h < 1.4

5.5 µm 15 µm 25 – 50 mL/h < 1.6

7.0 µm 21 µm 80 – 150 mL/h < 1.6

Application information To give an overview of the parameter settings best suited for a speciﬁc process, special training

papers can be downloaded directly from our webpage (www.buchi.com). For special applications please contact us.

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6.7 End of spray drying process

Caution

Risk of minor or moderate burning when handling hot parts.

• Do not touch hot parts

• Let the system cool down for some minutes after use

Finish a spray drying process

1. Switch off the heater by pressing the “Heat” button and let the system cool down. Depending on the environmental temperature, this may take several minutes.

2. Switch off the spray head by pressing the “Spray” button.

3. Stop the gas ﬂow at an inlet temperature below 70 °C.

4. Read the internal pressure of the Nano Spray Dryer B-90. No overpressure should be present.

5. Take out the pump inlet tube of the sample solution. The pump will now transport air, displacing product deposits in the tubing and spray head. Turn OFF the peristaltic pump afterwards and lower the pump bed to release the mechanical load of the pulleys at the tube.

6. See section 6.8 before open the glass assembly in safe environment prior to any particle recovery!

6 Operation

6.8 Collecting the particles from the collector cylinder

Danger

Death or serious poisoning by inhalation or incorporation of dried particles at recovery.

• Wear safety goggles

• Wear safety gloves

• Wear a suitable protective mask

• Wear a laboratory coat

• Do not inhale dried particles

• Stop drying gas ﬂow before opening the drying circuit

• Only recover particles in sufﬁciently ventilated ﬂue or glove-box

• Do not disperse the dried particles

• Do not clean dusty parts with compressed air

General information about particle recovery To recover the particles from the wall of the collecting electrode a particle scraper and collecting

paper can be used. It allows recovering the particles manually and deposits the particles on a sheet of weighing paper.

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6 Operation

The electrostatic particle collector has very high separation efﬁciency. Nevertheless some particles may be deposited on the glass cylinder wall and the inner star electrode. These particles can be recovered carefully with a spatula or a brush.

Recommended set of tools for particle recovery

• BUCHI particle scraper (order no. 11055338)

• BUCHI weighing paper in A4 format (order no. 11055339)

Particle recovery procedure

1. Place a blank sheet of weighing paper on a free area inside a fume hood.

2. Remove the collector cylinder from the bottom basement of the particle collector.

3. Place the collector cylinder on the sheet of paper.

4. Use a particle scraper to collect particles from the cylinder.

5. Lift the cylinder from the weighing paper and put it aside.

6. Fill the powder from the sheet of paper into a storage vessel. Depending on the substance, a particle recovery rate of up to 90 % can be achieved.

NOTE

Act carefully (e.g. avoid shaking movements) in order to prevent loss of particles. Clean all contaminated parts thoroughly to avoid hazardous situations and cross contamination. For information about cleaning, see section 7.6.

6.9 Other operation modes

6.9.1 Inert Loop B-295 operation

System preconditions

All system items must be correctly installed according to the set-up conﬁguration. See section 5 for more information. Carry out a ﬁnal installation check (see section 5.9) before starting a spray drying process.

Danger

Death by suffocation or serious poisoning by inhalation of inert gases.

• Do not inhale inert gases

• Directly withdraw released gases and gaseous substances by sufﬁcient ventilation

• Only operate the instrument in ventilated environments

• Before operation, check all parts, connections and sealings involved in the gasﬂow for proper sealing

• Exchange worn out or defective parts immediately

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Danger

Death or serious poisoning by gases or particles at O2– sensor or ﬁlter malfunction

• Exchange defective O2– sensor immediately

• Exchange O2– sensor regularly within the speciﬁed maintenance intervals

• Exchange clogged ﬁlters immediately

• Exchange ﬁlters regularly within the speciﬁed maintenance intervals

• Safely dispose ﬁlter immediately

Warning

Death or serious injuries by compressed gas.

• Depressurize gas circuit before any modiﬁcation work

• Wear safety goggles

6 Operation

Warning

Death or serious poisoning by contact or incorporation of condensed liquid.

• Dispose condensate after use safely

• Wear safety gloves

Inert Loop B-295 operation

1. Switch on the Inert Loop B-295 and the Nano Spray Dryer B-90.

2. Check the oxygen sensor by blowing ambient air through the instrument. The Ambient oxygen concentration should be around 21 %.

3. Select the gas mode (~4 % O2 or ~1 % O2) in submenu 1: The instrument automatically detects the connected periphery.

4. Switch on the Aspirator.

5. Turn on the inert gases N2 and CO2. Set the CO2 pressure to maximal 2 bar and the absolute N2 pressure below 1.3 bar.

6. Switch on the heater by pressing the “Heat” button and wait until the system has reached stationary temperature conditions (typically after 5 to 10 min.).

7. Turn on the peristaltic pump to supply the spray head with a pure organic solvent test solution on base of the target sample solution.

8. Press the “Spray” button, the system switches on the high voltage at the collecting electrode. The inert gas ﬂow starts working together with the spray head. As soon as the inert gas mixture has reached optimal processing values, the spray LED starts blinking.

9. Press the “Spray” button again to conﬁrm. The system is now ready for the spray drying process.

10. Change from the solvent solution to the product solution while the system is still spraying.

11. If a setup with the Dehumidiﬁer B-296 is used, switch on the Dehumidiﬁer B-296 at the same time as the Inert Loop B-295.

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NOTE

Inert gas pressure above the values (see Inert Loop B-295 operation, step 5) will activate the safety pressure relief valve, causing inert gas loss.

Aqueous solutions or mixtures of organic solutions and water may freeze in the heat 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.

A leaking Aspirator can cause high O2 concentrations in ‘closed loop’. If the concentration is considerably high, stop spray drying process and check Aspirator for leakages immediately.

6.9.2 Dehumidiﬁer B-296 operation

The Dehumidiﬁer B-296 can be used in ‘open loop’ or in ‘closed loop’ conﬁguration in combination with the Nano Spray Dryer B-90.

Warning

Death or serious poisoning by contact or incorporation of condensed liquid.

• Dispose of condensate safely after use

• Wear safety gloves

6 Operation

System preconditions All system items must be correctly installed according to the kind of set-up, see section 5 for more

information. Carry out a ﬁnal installation check (see section 5.9) before every spray drying process! Operate the Nano Spray Dryer B-90 Advanced in ‘closed loop’ as follows

1. Switch on the Nano Spray Dryer B-90 Advanced.

2. Only in ‘closed loop’ conﬁguration, plug the dongle into the Nano Spray Dryer B-90 (see section

4.10; socket c).

3. Check the oxygen sensor with ambient air. The Ambient oxygen concentration should be around 21 %.

4. Select the inert gas mode (~4 % O2 or ~1 % O2) in “submenu 1”. The instrument automatically detects the connected dongle.

5. Turn on the inert gases N2 and CO2. Set the CO2 pressure to maximal 2 bar and the absolute N2 pressure below 1.3 bar.

6. Switch on the Dehumidiﬁer B-296.

7. Switch on the Aspirator.

8. Switch on the heater by pressing the “Heat” button and wait until the system has reached stationary temperature conditions (typically after 5 to 10 min.).

9. Turn on the peristaltic pump to supply the spray head with a pure organic solvent test solution on base of the target sample solution.

10. Press the “Spray” button, the system switches on the high voltage at the collecting electrode. The inert gas ﬂow starts working together with the spray head. As soon as the inert gas mixture has reached optimal processing values, the spray LED starts blinking.

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11. Press the “Spray” button again to conﬁrm. The system is now ready for the spray drying process.

12. Change from the solvent solution to the product solution while the system is still spraying.

NOTE

Before switching from one organic solvent solution to another it is highly recommended to dry the working ‘closed loop’ by running the aspirator with dry air for half an hour. This will lower the possibility of cross contamination signiﬁcantly.

6.10 Using the Nano Spray Dryer Records software on a PC

The PC-software enables online data monitoring and storage of experimental runs in a virtual library.

Functionality

• Documentation of process data of experimental runs

• Export of process parameters for further data analysis

Connecting the instrument to the PC Connect the Nano Spray Dryer B-90 to the PC by means of the USB cable. Insert the CD into the PC

and follow the descriptions on the CD for system requirements and software installation.

6 Operation

Starting the program

Double click on the program icon to start Nano Spray Dryer Records.

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Initial view and program functions

6 Operation

Menu bar entries: Accessible sub entries:

File • New LabBook

• Open LabBook

• Close LabBook

• Exit

View • Show tree

Tools • Selftest

• Options

Help • Contents

• Import License

• Software registration

• About

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Tool bar functionality

a b c d e f g h i j k l

Tool bar items: Tool functionality:

6 Operation

LabBook entries Each experiment is stored as an entry in a LabBook. In order to record an experiment a LabBook

must already be available or has to be created ﬁrst.

Start/Stop recording

New LabBook

Delete LabBook

Open existing LabBook

Close LabBook

Import LabBook

Export LabBook

Open Experiment

Show Report (Create a pdf-ﬁle with a choosen data set)

Export to CSV (Character-Separated Values)

Close Experiment

Delete Experiment

• Click the button “New LabBook”, a small pop-up window appears (see screenshot above). Name

the LabBook and click “create”. The new LabBook will appear in the left tree area of the program screen.

• Press the “Start/Stop recording” button to acquire online process data while the Nano Spray

Dryer B-90 is switched on.

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Program options The program can be conﬁgured in the “Options” menu.

6 Operation

• Select the appropriate data recording rate and storage interval

• Select the units of temperature, pressure and gas ﬂow

• Choose the language of the user interface (default is English)

• Upload a company logo and change displayed company name on PDF reports

• Activate check boxes to set startup view

NOTE

Any changes made under “Options” will be applied after a restart of the program.

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6 Operation

Experiment metadata LabBooks can be equipped with additional metadata for each experiment. These metadata can hold

comments, unique attributes for identiﬁcation and information about the drying conditions and system settings. This information will show up in PDF reports.

• Select a LabBook and one or more experiment entries. Activated experiments will appear in the

tree area on the left.

• Click on a single experiment entry at the tree area. Metadata can now be manipulated.

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Access recorded data Recorded spray drying data can be displayed in plot or table view.

6 Operation

All main spray drying process parameters like inlet and outlet temperatures, pressure and gas ﬂow are recorded and visualized in the “Plot View”. The plots can be zoomed-in via mouse action. Use the computer mouse to mark an area of interest on a plot. Release the mouse button to zoom into the area.

All other actual process data can be read out in the time based “Table View”. Click on the column headers to sort the table.

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6 Operation

Data export

• Experiments can be exported into a CSV ﬁle. To export an experiment click the “Export to CSV”

button. Subsequently name and save the ﬁle on a ﬁle system.

• PDF reports can be generated from experiments via the “Show Report” button. This ﬁle can be

named and saved on a ﬁle system.

Run a self-test of the Nano Spray Dryer B-90 The software provides a self-test function to report the actual condition of the Nano Spray Dryer B-90.

The self-test instructions and procedures are displayed on the screen of the Nano Spray Dryer B-90. At the end of the self-test, a PDF report is generated. It can be used as a support tool by BUCHI representatives for service and trouble shooting.

NOTE:

The serial number of the Nano Spray Dryer B-90 is requested during the self-test. It can be found on the name plate on the back side of the instruments housing.

Software licensing The software can be validated for 60 days. At the end of this period the software will request a license

ﬁle to stay functional.

1. Fill out the Software Registration Form under Help.

2. The form generates an XML ﬁle. Send this ﬁle to your local BUCHI representative to receive a validated license ﬁle (*.lic) in return.

3. Import the license ﬁle via “Help”>”Import License”

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7 Maintenance and repairs

This chapter gives instructions on maintenance work to be performed in order to keep the instrument in a good and safe working condition. All maintenance and repair work requiring the opening or removal of the instrument housing must be carried out by trained personnel and only with the tools provided for this purpose.

NOTE

Use only genuine consumables and spare parts for any maintenance and repair work in order to assure warranty and continued system performance. Any modiﬁcations of the Nano Spray Dryer B-90 or parts of it need prior written permission of the manufacturer.

Danger

Death or serious poisoning by inhalation or incorporation of dried particles during maintenance.

• Wear safety goggles

• Wear safety gloves

• Wear a suitable protective mask

• Wear a laboratory coat

• Clean all parts thoroughly

• Only maintain the instrument in ventilated environments

• Do not inhale dried particles

• Stop drying gas ﬂow before opening the drying circuit

7 Maintenance and repairs

Warning

Death or serious burning by electric current.

• Switch off the instrument, disconnect the power cord and prevent unintentional restart before removing housing or parts of it

• Do not touch parts inside the instrument with wet hands

• Do not spill liquids over electronic components

• Do not squeeze cables, tubes or other items at reassembling

• Exchange defective cabling or tubing before reassembling

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Warning

Death or serious injuries by compressed air and gases.

• Depressurize air and gas circuit ﬁrst

• Wear safety goggles

7 Maintenance and repairs

Risk of instrument and instrument damage by liquids and detergents.

• Do not spill liquids over the instrument or parts of it

• Wipe off any liquids instantly

• Use ethanol or soapy water as detergent only

7.1 Customer service

Only authorized service personnel are allowed to perform repair work on the instrument. Authorization requires a comprehensive technical training and knowledge of possible dangers which might arise when working at the instrument. Such training and knowledge can only be provided by BUCHI.

Addresses of ofﬁcial BUCHI customer service ofﬁces are given on the BUCHI website under: www.buchi.com. If malfunctions occur on your instrument or you have technical questions or application problems, contact one of these ofﬁces.

The customer service offers the following:

• Spare part delivery

• Repairs

• Technical advice

Notice

7.2 Housing condition

Check the housing for visible defects (switches, plugs, cracks) and clean it regularly with a damp cloth.

7.3 Glass component conditions

Clean the glass components after each spray process to prolong the lifetime. The glass assemblies can be taken out and cleaned manually with water and a commercial cleaning agent (e.g. mild soap solution) or in an ultrasonic bath. Visibly check for damages at all the glass components subsequently.

NOTE

• It is recommended to clean all glass components.

• Regularly check the glassware components for damage and use only glassware in perfect condition, i.e. glassware without cracks or stars.

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Risk of minor or moderate cuts when handling damaged glass parts.

• Handle glass parts with care

• Visually inspect every glass part before mounting

• Exchange damaged glass parts immediately

• Do not touch cracks or bits of broken glass with bare hands

7.4 Oxygen sensor

The live time of the oxygen sensor in the Nano Spray Dryer B-90 Advanced or Inert Loop B-295 is approx. 1.5 years. Replace the sensor after this period or in case of malfunction. To remove the sensor disconnect the sensor cabling and unscrew it by turning it anticlockwise. For installation proceed in reverse order.

7.5 Sealing conditions

7 Maintenance and repairs

Caution

All sealings are recommended to be checked yearly. When replacing the seals, take care not to damage them.

• To prevent damaging the seals never apply grease and never touch them with sharp objects.

• To prolong the lifetime of the seals, rinse them routinely with water or ethanol and always when

there has been the possibility of unwanted sample contamination.

• Dry the cleaned seals with a soft, lint-free cloth.

7.6 Cleaning

The following subsections describe possible cleaning actions. All actions should be performed regularly and thoroughly.

7.6.1 Spray head and tube connections

Clean the feed tubing and the spray head after every spray process.

• To clean the central hole of the spray head body use water.

• Rinse the spray caps routinely with water or ethanol for primary cleaning.

• Recommended: Cleaning of the spray cap mesh in an ultrasonic bath.

Caution

Risk of minor or moderate burning when handling hot parts.

• Do not touch hot parts

• Let the system cool down for some minutes after use

NOTE

For maximum throughput and to avoid cross contamination of the spray drying output it is essential to work with a clean spray cap and tube assembly! Total cleaning of the spray caps (in particular cleaning of the micropore meshes) needs an ultrasonic bath processing for about 10 minutes.

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7.6.2 Outlet ﬁlter

A clogged outlet ﬁlter results in a pressure drop between inside the Nano Spray Dryer B-90.

7 Maintenance and repairs

Risk of instrument damage by internal overpressure.

• External supply pressure must meet the system speciﬁcations

• Exchange clogged ﬁlters immediately

• Safely dispose ﬁlter immediately

• If the pressure drops by more than 20 mbar relative to a clean outlet ﬁlter, take the ﬁlter out and

wash it manually or in a laboratory washing machine.

• Replace the outlet ﬁlter annually or if damaged.

7.6.3 Inert Loop B-295 and Dehumidiﬁer B-296

The sealed working circuits of the devices and the optional heat exchanger in combination with the Inert Loop B-295 can be ﬂooded completely for cleaning purpose.

Risk of instrument and instrument damage by liquids and detergents.

• Do not spill liquids over the instrument or parts of it

• Wipe off any liquids instantly

• Use ethanol or soapy water as detergent only

Notice

• Switch off all relevant devices and unplug the respective power cords.

• Remove the molecular sieve bag for the duration of cleaning if installed.

• Check all sealings and tubes for good condition and proper sealing.

• Raise the exhaust tube and ﬁll the system through the inlet with cleaning medium (e.g. ethanol).

• Provide a collection vessel to collect the cleaning medium ﬂowing from the system. Open the drain

valve and lower the exhaust tube, so that the cleaning medium ﬂows out.

• Rinse out and dry the condensate vessel.

• Reinstall the condensate vessel.

• To dry the working circuit connect the Nano Spray Dryer B-90 and dry it by running the Aspirator

with dry air.

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8 Troubleshooting

This chapter helps to resume operation after a problem has occurred with the instrument which does not require special technical training. 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 “Remedy”. Malfunctions or errors which are not listed in the table are to be corrected by a BUCHI trained technical engineer who has access to the ofﬁcial 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

Error number Error reading Possible cause Remedy

8 Troubleshooting

001 Temperature sensor

spray head not connected

003 Resonance not found

check the spray head

005 Spray head temperature

exceeded

007 Temperature sensor

outlet not connected

008 Temperature sensor

inlet not connected

Defective sensor, sensor cable or internal wiring

No spray nut, spray nut not tight enough, spray head defective

Piezo defective, temperature problem

Defective sensor, sensor cable or internal wiring

Check if the spray head plug is plugged in correctly. Switch off the device and try again. If the error still occurs replace the spray head or contact the BUCHI customer service.

Switch off the device and try again, if the error still occurs clean the spray cap, replace the spray cap, replace the spray head or contact the BUCHI customer service.

Switch off the device and try again. If the error still occurs replace the spray head or contact the BUCHI customer service.

Switch off the device and try again. Check if the outlet temperature sensor is plugged in correctly. If the problem still occurs replace the outlet temperature sensor or contact the BUCHI customer service.

Switch off the device and try again. Check if the inlet temperature sensor is plugged in correctly. If the problem still occurs replace the inlet temperature sensor or contact the BUCHI customer service.

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8 Troubleshooting

Table 8-1: Error messages and their remedy (cont.)

011 Inlet temperature exceeded Heating control or heating relais

defective

014 Voltage HV-Module HV-module defect or internal

wiring interruption or quality falloff voltage because of a short circuit

015 Current in HV-Module too high HV-module defect or internal

wiring interruption

016 Current in HV-Module too low HV-connector not plugged in or

defective wiring error

020 Relative pressure sensor 1

not connected

021 Relative pressure sensor 2

not connected

023 Difference pressure sensor

not connected

024 Inside pressure low System not leakproof Test for leaks

025 Filter pressure drop low Filter not installed or defective

026 Flow rate low No ﬂow rate, system not leak-

027 Inside pressure high Gas pressure connection too

028 Flow rate high Sensor is at stop position Reduce gas ﬂow rate

029 Relative pressure sensor 1

defective

030 Relative pressure sensor 2

defective

032 Difference pressure sensor

defective

035 No glass isolation cylinder Position switch Install glass insolation cylinder

040 Valve 1 CO2

not connected

041 Valve 2 O2

not connected

042 O2 sensor not connected Defective sensor, sensor cable or

Sensor not connected or defective internal wiring

internal wiring

proof

high

Sensor or internal wiring defective

Internal wiring defective or missing

internal wiring

Switch off the device and try again. If the error still occurs replace the heater module or contact the BUCHI customer service.

Switch off the device and try again. If the error still occurs contact the BUCHI customer service.

Switch off the device and try again. Check the HV-module, connection. If the error still occurs , contact the BUCHI customer service.

Contact BUCHI customer service

Contact BUCHI customer service BUCHI

Check if outlet ﬁlter is blocked. Replace the ﬁlter.

Generate gas ﬂow, test for leaks

Regulate gas pressure

Contact BUCHI customer service

Close gas ﬂow rate and restart the system, contact BUCHI customer service

Contact BUCHI customer service

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8 Troubleshooting

Table 8-1: Error messages and their remedy (cont.)

043 O2 sensor short-circuit Defective sensor, sensor cable or

internal wiring

046 O2 concentration high System not leakproof, N2-bottle

empty

047 O2 concentration low Valve defective Contact BUCHI customer service

050 B-295 O2 concentration

too high

051 Change gas mode Electrical communication cable

058 EEPROM Contact BUCHI customer service.

Only for operation with the Inert Loop B-295

System not leakproof, N2-bottle empty

B-290 / B-295 or dongle not connected

Contact BUCHI customer service

Test for leakages. Check system sealings and N2-supply.

Check cabling or dongle.

200 Connection to B-295 interrupted

or disconnected

201 B-295 plugged in while opera-

tion in process

203 Pressure alarm not given during

start-up

204 Failure cooling unit B-295 Contact BUCHI customer service.

8.2 Malfunctions and their remedy

Table 8-2: Malfunctions and their remedy

Malfunction Possible cause Remedy

Equipment cannot be switched on No voltage Insert mains plug, examine plug for

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

System does not heat up Heater cable not plugged in Plug in heating circuit

Defective connection cable or instrument is not plugged in

Connection cable plugged in after switching on the instrument

Pressure switch defective or contaminated

Fuse has been activated Reset fuse manually

running surface

Heating is not switched on Switch on heat

Nominal entry temperature is below room temperature

Fuse has been activated Reset fuse manually

Heater defective Contact the BUCHI customer service

Faulty gas ﬂow direction or no ﬂow in the heating system

Check connection cable for damage and insert plug.

Restart the system.

Contact BUCHI customer service.

damage

Elevate the running surface with the lever. Adjust the lifting height of the running surface with the hexagonal hex-wrench from beneath

Re-select a new inlet temperature

Check pipe system

89 B-90 Operation Manual, Version B

8 Troubleshooting

Table 8-2: Malfunctions and their remedy (cont.)

Spray head blocked Product is too concentrated Use a lower sample concentration

Change to a bigger spray cap / mesh

Clean the spray head and spray cap

Product drips in spray cylinder No spray ﬂow Turn on spray

Insufﬁcient spray ﬂow Inspect inside gas pressure

(20-50 mbar) and gas supply

Deposits on the spray cylinder Spray head is not clean Completely dismantle the spray head

and clean with water

Spray head is defective (bent PEEK tubing, washer or mesh)

Product will not dry Increase inlet temperature

Inlet temperature is above the melting point of the product

Product related deposits No action possible

Irregular or pulsed spraying Leaks in the spray head Check seal in the spray head and

Deposits in the particle collector Product too moist Increase inlet temperature to dry the

Inlet temperature falls Heating is switched off Switch on heating

Heater plug is unplugged Insert heater plug

Outlet temperature falls No heating Follow measures under “Fall of entry

Spraying too powerful Reduce production rate of spray

Outlet temperature rises System has not reached stationary

temperature conditions

Spray head blocked Clean the spray head

Feed tubing not dipped into sample solution

Change of concentration in sample solution

No feed of product Switch on peristaltic pump

Replace spray cap or defective element

Reduce inlet temperature

replace if necessary

product

Increase residence time of product in drying cylinders

Increase gas ﬂow rate to increase the energy input for drying

temperature”

Warm up the system with hot drying gas for about 30 minutes.

Dip feed tubing into product

Agitate product (magnetic stirrer) to obtain uniform concentration

90 B-90 Operation Manual, Version B

9 Shutdown, storage, transport and disposal

This chapter instructs how to shut down and to pack the instrument for storage or transport. Speciﬁcations for storage and shipping conditions can also be found listed here.

9.1 Storage and transport

Switch off the instrument and remove the power cord. To disassemble the Nano Spray Dryer B-90 follow the installation instructions in section 5 in reverse order. Remove all liquids and dusty residues before packaging the instrument.

Warning

Death or serious poisoning by contact or incorporation of harmful substances.

• Wear safety goggles

• Wear safety gloves

• Wear a suitable protective mask

• Wear a laboratory coat

• Clean the instrument and all accessories thoroughly to remove possibly dangerous substances

• Do not clean dusty parts with compressed air

• Store the instrument and its accessories at a dry place in its original packaging

Caution

Risk of minor or moderate injury by heavy weight of the instrument.

• Consult a second person to transport the instrument

• Do not drop the instrument

• Place the instrument on a stable, even and vibration-free surface

• Keep limbs out of crushing zone

91 B-90 Operation Manual, Version B

9.2 Disposal

For instrument disposal in an environmentally friendly manner, a list of materials is given in chapter 3. This helps to ensure that the components can be separated and recycled correctly. You have to follow valid regional and local laws concerning disposal. For help, please contact your local authorities!

NOTE

When returning the instrument to the manufacturer for repair work, please copy and complete the health and safety clearance form on the following page and enclose it with the instrument.

9 Shutdown, storage, transport and disposal

92 B-90 Operation Manual, Version B

9 Shutdown, storage, transport and disposal

Health and Safety Clearance

Declaration concerning safety, potential hazards and safe disposal of waste.

For the safety and health of our staff, laws and regulations regarding the handling of dangerous goods, occupational health and safety regulations, safety at work laws and regulations regarding safe disposal of waste, e.g. chemical waste, chemical residue or solvent, require that this form must be duly completed and signed when equipment or defective parts were delivered to our premises.

Instruments or parts will not be accepted if this declaration is not present.

Equipment

Model: Part/Instrument no.:

1.A Declaration for non dangerous goods

We assure that the returned equipment

has not been used in the laboratory and is new was not in contact with toxic, corrosive, biologically active, explosive, radioactive or

other dangerous matters.

is free of contamination. The solvents or residues of pumped media have been

drained.

1.B Declaration for dangerous goods

List of dangerous substances in contact with the equipment:

Chemical, substance Danger classification

We assure for the returned equipment that

all substances, toxic, corrosive, biologically active, explosive, radioactive or

dangerous in any way which have pumped or been in contact with the equipment are listed above.

the equipment has been cleaned, decontaminated, sterilized inside and outside and

all inlet and outlet ports of the equipment have been sealed.

2. Final Declaration

We hereby declare that

- we know all about the substances which have been in contact with the equipment and all questions have been answered correctly

- we have taken all measures to prevent any potential risks with the delivered equipment.

Company name or stamp:

Place, date:

Name (print), job title (print):

Signature:

Health and Safety Clearance_20081110.doc_20081110 Version 1.0 Page 1/1

93 B-90 Operation Manual, Version B

10 Spare parts

This chapter lists spare parts, accessories and options including their ordering information. Only order spare parts and consumables from BUCHI to maintain the warranty status and to assure best performance and reliability of the system and affected components. Any modiﬁcations to the spare parts used are only allowed with the prior written permission of the manufacturer.

Always state the product designation, instrument serial and part numbers for warranty clearance when ordering spare parts!

10.1 Spray head

Table 10-1: Spray head

Description Order no.

10 Spare parts

Spray head 051510

Spray head holder 051508

Set of 3 spray caps 4.0 µm 051747

Set of 3 spray caps 5.5 µm 051748

Set of 3 spray caps 7.0 µm 051749

Set of 5 feed tubings for spray head 11055830

Set of feed tubing connections 051768

Set of 20 o-rings EPDM for spray cap 051772

Set of 20 o-rings HITECH-HRC-75 for spray cap 11055795

Fittings D1/16’’ gray (25 pieces) 044816

Ferrules D1/16’’ gray (25 pieces) 044269

Set of silicone seals (20 pieces) 040023

Connecting screw cap GLS 80 051518

Closing screw cap GLS 80 051529

94 B-90 Operation Manual, Version B

10.2 Glass parts and mounting items

10 Spare parts

Table 10-2: Glass parts and mounting parts

Description Order no.

Spray cylinder 051511

Glass cylinder 051549

Sealing set complete 051778

Tool box B-90 051767

Centerpiece holder 051630

Support metal bar 051575

95 B-90 Operation Manual, Version B

10.3 Particle collector, heater and lifting device items

Table 10-3: Electrical particle collector, heater and

Description Order no.

Particle collecting tube 051662

Glass insulation tube 051663

Collector base complete 051669

Nano particle scraper 11055338

Particle collection paper (100 pages) 11055339

10 Spare parts

lifting device

Heater complete 051504

Set of 3 polyethylene frits with sealing ring 051777

Temperature sensor PT-1000 051766

High voltage star electrode protected 11055174

Protective grid 051680

Plastic distance sheet 051530

Lifting device 051607

96 B-90 Operation Manual, Version B

10.4 Filters

10 Spare parts

Table 10-4: Outlet ﬁlter

Description Order no.

Outlet ﬁlter 051656

Table 10-5: Inlet ﬁlter

Description Order no.

Inlet ﬁlter complete 011235

Replacement ﬁlter with seal 011238

Tube Flexﬂyte D51mm (0.8 m) 011240

10.5 Tubing and accessories

Table 10-6: Tubing

Description Order no.

Gas inlet connection 051781

Polypress tube gas outlet (2 m) 046329

Hose clamp 25-40mm 004236

Pressure relieve valve 11055829

Polypress tube quick coupling 045656

Compressed gas tube complete 046356

Compressed gas hose coupling 5.5mm 044407

Hose Solaﬂex 13.5/8 mm 004113

Hose clamp 10-16 mm 022352

Upgr. set B-90 Advanced for closed cycle

11055748

(service engineer required for installation)

Oxygen Sensor 046348

Set of internal B-90 tubings complete 051790

Silicone tube for heater (1.3 m and 2.0 m) 11055794

97 B-90 Operation Manual, Version B

Table 10-6: Tubing (cont.)

Peristaltic pump complete 051735

Silicone feed tubing (per m) 004138

Tygon tubing MH 2075 transp. (per m) 046314

Tygon tubing F 4040 A yellow (per m) 046315

Tube Cutter 019830

PC software Nano Spray Dryer records 051776

USB Kabel 2.0 A-B (2.0 m) 11055310

USB Kabel 2.0 A-B (4.5 m) 049226

10.6 Inert Loop B-295, Dehumidiﬁer B-296 and Adsorption Column

10 Spare parts

46348

04105 27338

40398

Table 10-7: Inert Loop B-295, Dehumidiﬁer B-296

and Adsorption column

Description Order no.

Receiving vessel for solvent, complete 040398

PTFE tube to receiving vessel 004105

PTFE hose connection SVL 22 027338

Oxygen sensor 046348

Upgrade set B-295 for closed cycle 051783

98 B-90 Operation Manual, Version B

10 Spare parts

Table 10-7: Inert Loop B-295, Dehumidiﬁer B-296

and Adsorption column (cont.)

Description Order no.

Upgrade set B-296 for closed cycle 051780

a Woulff bottle 041875

b Screw cap SVL 22 003577

c Closed screw cap SVL 22 005222

Gasket 22×17 PTFE 005155

PFTE hose connection SVL 22 027338

Polypress tube (2m) 046329

Hose clamp 25-40 mm 004236

Viton seal for product collect vessel 040471

Connecting piece for tube 044679

Screw cap SVL 42 003551

Closed screw cap SVL 42 046357

Seal SVL 42×30 PTFE 003575

FEP nipple 018916

Screw cap GL14 033577

99 B-90 Operation Manual, Version B

11 Declarations and requirements

11.1 FCC requirements (for USA and Canada)

English: This equipment has been tested and found to comply with the limits for a Class A digital device,

pursuant to both Part 15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communications. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment. This equipment generates, uses and can radiate radio frequency energy and, if not installed and used in accordance with the instruction manual, may cause harmful interference to radio communications. Operation of this equipment in a residential area is likely to cause harmful interference in which case the user will be required to correct the interference at his own expense.

Français: Cet appareil a été testé et s’est avéré conforme aux limites prévues pour les appareils numériques

de classe A et à la partie 15 des réglementations FCC ainsi qu’à la réglementation des interférences radio du Canadian Department of Communications. Ces limites sont destinées à fournir une protection adéquate contre les interférences néfastes lorsque l’appareil est utilisé dans un environnement commercial. Cet appareil génère, utilise et peut irradier une énergie à fréquence radioélectrique, il est en outre susceptible d’engendrer des interférences avec les communications radio, s’il n’est pas installé et utilisé conformément aux instructions du mode d’emploi. L’utilisation de cet appareil dans les zones résidentielles peut causer des interférences néfastes, auquel cas l’exploitant sera amené à prendre les dispositions utiles pour palier aux interférences à ses propres frais.

11 Declarations and requirements

100 B-90 Operation Manual, Version B

BUCHI B-90 User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual