Buchi MiniSprayDryer S-300 Manual
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MiniSprayDryer S-300
Operation Manual
Imprint
Product Identification:
Operation Manual (Original) MiniSprayDryer S-300
11594255
Publication date: 08.2022
Version A
BÜCHI Labortechnik AG
Meierseggstrasse 40
Postfach
CH-9230 Flawil 1
E-Mail: [email protected]
BUCHI reserves the right to make changes to the manual as deemed necessary in the light of experience, especially with respect to structure, illustrations and technical details.
This manual is copyrighted. Information from it may neither 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.
Büchi Labortechnik AG Table of contents
Table of contents
Operation Manual MiniSprayDryer S-300 iii
Table of contents Büchi Labortechnik AG
iv Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG Table of contents
Preparing the outlet filter with PTFE membrane (Option)....................................... 37
Preparing the peristaltic pump for auto mode (option) ........................................... 43
Preparing the product temperature sensor (option)................................................ 44
Operation Manual MiniSprayDryer S-300 v
Table of contents Büchi Labortechnik AG
vi Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG Table of contents
Operation Manual MiniSprayDryer S-300 vii
1 | About this document
1
1.1
1.2
1.3
Büchi Labortechnik AG
About this document
This operation manual is applicable for all variants of the instrument.
Read this operation manual before operating the instrument and follow the instructions to ensure safe and trouble-free operation.
Keep this operation manual for later use and pass it on to any subsequent user or owner.
BÜCHI Labortechnik AG accepts no liability for damage, faults and malfunctions resulting from not following this operation manual.
If you have any questions after reading this operation manual: u
Contact BÜCHI Labortechnik AG Customer Service.
https://www.buchi.com/contact
Mark-ups and symbols
NOTE
This symbol draws attention to useful and important information.
R This character draws attention to a requirement that must be met before the instructions below are carried out.
u
This character indicates an instruction that must be carried out by the user.
ð This character indicates the result of a correctly carried out instruction.
Mark-up
Window
Explanation
Software Windows are marked-up like this.
Tab
Tabs are marked-up like this.
Dialogs are marked-up like this.
Dialog
[Button]
[Field names]
[Menu / Menu item]
Status
Signal
Buttons are marked-up like this.
Field names are marked-up like this.
Menus or menu items are marked-up like this.
Status is marked-up like this.
Signals are marked-up like this.
Trademarks
Product names and registered or unregistered trademarks that are used in this document are used only for identification and remain the property of the owner in each case.
Connected devices
In addition to these operating instructions, follow the instructions and specifications in the documentation for the connected devices.
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2
2.1
2.2
2.3
Safety | 2
Safety
Proper use
The instrument is designed for spray drying.
The instrument can be used in laboratories for the following tasks:
Spray drying
Use other than that intended
The use of the instrument other than described in proper use and specified in technical data is use other than that intended.
The operator is responsible for damages or hazards that are caused by use other than that intended.
Specially the following uses are not permitted:
Use of the instrument with non-BUCHI products.
Use of the instrument in closed mode with non-certified instruments.
Use of the instrument in an environment with a potential risk of explosion or areas which require explosion-safe apparatus.
Use of the instrument without an appropriate leading away exhaust gas from the working area.
Use of the instrument with gases with unknown chemical composition.
Use of the instrument with organic solvents (> 20 %) without Inert Loop.
Use of the instrument with organic solvents (> 20 %) in open mode.
Use of the instrument with samples containing peroxides.
Use of the instrument with samples that can form peroxides.
Use of the instrument with samples which produce oxygen during the processing.
Use of the instrument with toxic substances without appropriate safety measures.
Use of the instrument with biohazardous materials such as viruses or hazardous bacteria.
Use of the instrument with samples which can block the feed channel of the nozzle.
Use of the instrument with substances which might explode or ignite because of the processing.
Use of the instrument with substances which might explode or ignite because of the selected parameters.
Use of the instrument with corrosive samples in closed mode.
Use of the instrument with corrosive samples other than the corrosive instrument version.
Use of the instrument with any other Inert Loop than the S-395 without the O2
box. See Chapter 12.2.2 "Accessories", page 80
Staff qualification
Unqualified persons are unable to identify risks and are therefore exposed to greater dangers.
Operation Manual MiniSprayDryer S-300 9/90
2 | Safety
2.4
2.5
Büchi Labortechnik AG
The instrument may only be operated by suitably qualified laboratory staff.
These operating instructions are aimed at the following target groups:
Users
Users are persons that meet the following criteria:
They have been instructed in the use of the instrument.
They are familiar with the contents of these operating instructions and the applicable safety regulations and apply them.
They are able on the basis of their training or professional experience to assess the risks associated with the use of the instrument.
Operator
The operator (generally the laboratory manager) is responsible for the following aspects:
The instrument must be correctly installed, commissioned, operated and serviced.
Only suitably qualified staff may be assigned the task of performing the operations described in these operating instructions.
The staff must comply with the local applicable requirements and regulations for safe and hazard-conscious working practices.
Safety-related incidents that occur while using the instrument should be reported to the manufacturer ([email protected]).
BUCHI service technicians
Service technicians authorized by BUCHI have attended special training courses and are authorized by BÜCHI Labortechnik AG to carry out special servicing and repair measures.
Personal protective equipment
Depending on the application, hazards due to heat and/or corrosive chemicals may arise.
u
Always wear appropriate personal protective equipment such as safety goggles, u protective clothing and gloves.
Make sure that the personal protective equipment meets the requirements of the safety data sheets for all chemicals used.
Warning notices in this document
Warning notices warn you of dangers that can occur when handling the instrument.
There are four danger levels, each identifiable by the signal word used.
Signal word
DANGER
WARNING
CAUTION
Meaning
Indicates a danger with a high level of risk which could result in death or serious injury if not prevented.
Indicates a danger with a medium level of risk which could result in death or serious injury if not prevented.
Indicates a danger with a low level of risk which could result in minor or medium-severity injury if not prevented.
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2.6
Safety | 2
Signal word
NOTICE
Meaning
Indicates a danger that could result in damage to property.
Warning symbols
The following warning symbols are displayed in this operation manual or on the instrument.
Symbol Meaning
General warning
Device damage
Dangerous electrical voltage
Hot surface
2.7
Fig. 1: Location of the warning symbols
Residual risks
The instrument has been developed and manufactured using the latest technological advances. Nevertheless, risks to persons, property or the environment can arise if the instrument is used incorrectly.
Appropriate warnings in this manual serve to alert the user to these residual dangers.
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2 | Safety Büchi Labortechnik AG
2.7.1
Faults during operation
If an instrument is damaged, sharp edges, moving parts or exposed electrical wires can cause injuries.
u u u
Regularly check instruments for visible damage.
If faults occur, switch off the instrument immediately, unplug the power cord and inform the operator.
Do not continue to use instruments that are damaged.
2.7.2
Hot surfaces
The surfaces of the device can become very hot. If touched they can cause skin burns.
u
Do not touch hot surfaces or else wear suitable protective gloves.
2.7.3
Dangerous vapors
The use of the instrument can produce dangerous vapors that are capable of causing life-threatening toxic effects.
u u u u u u
Do not inhale any vapors produced during processing.
Ensure that vapors are removed by a suitable fume hood.
Only use the device in well ventilated areas.
If vapors escape from connections, check the seals concerned and replace them if necessary.
Do not process any unknown fluids.
Observe the safety data sheets for all substances used.
2.7.4
Dangerous particles
The use of the instrument can produce dangerous particles that can cause lifethreatening toxic effects.
u
Do not inhale any particles produced during processing.
u u
Ensure that particles are removed by a suitable fume hood.
Only use the instrument in well ventilated areas.
u
If particles escape from connections, check the seals concerned and replace them if necessary.
u u
Do not process any unknown fluids.
Observe the safety data sheets for all substances used.
2.7.5
Glass breakage
Broken glass can cause severe cuts.
Damaged glass components may implode if subjected to a vacuum.
Minor damage to the ground joints impairs the sealing effect and may therefore diminish performance.
u u
Handle the flask and other glass components carefully and do not drop them.
Always visually inspect glass components for damage every time they are to be u u used.
Do not continue to use glass components that are damaged.
Always wear protective gloves when disposing of broken glass.
2.7.6
Malfunction of a connected instrument (option)
A malfunction on a connected instrument can cause poisoning or death.
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2.8
Safety | 2 u
Make sure that the connected instrument is prepared and maintained according to the user documentation.
Modifications
Unauthorized modifications can effect safety and lead to accidents.
u
Use only genuine BUCHI accessories, spare parts and consumables.
u u
Carry out technical changes only with prior written approval from BUCHI.
Only allow changes to be made by BUCHI service technicians.
BUCHI accepts no liability for damage, faults and malfunctions resulting from unauthorized modifications.
Operation Manual MiniSprayDryer S-300 13/90
3 | Product description
3
3.1
Büchi Labortechnik AG
Product description
Description of function
Spray drying is a processing technology to transform a liquid feedstock into a dried powder through four fundamental steps:
Atomization of the feed into a spray
Spray gas contact
Solvent evaporation
Separation of the dried product from the drying medium
The following spray drying modes are available:
Spray drying mode
Open mode
Closed mode with Inert Loop
(When using Ultrasonic Package accessory inert gas adapter is necessary)
Closed mode with Inert Loop and Dehumidifier
(When using Ultrasonic Package accessory inert gas adapter is necessary)
Solvent composition up to 20 % organic solvent between 90 % - 100 % organic solvent between 20 % - 80 % organic solvent
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3.2
Configuration
Product description | 3
Operation Manual MiniSprayDryer S-300 15/90
3 | Product description
3.2.1
Front view
Büchi Labortechnik AG
1 2 3 4
16/90
22
21
20
19
18
5
6
7
8
9
10
11
17 16
Fig. 2: Front view
1 Switch valve
(Advanced and Corrosive only)
3 Plug peristaltic pump 2
5 Interface
See Chapter 6 "Interface", page 29
15
7 Inlet from filter / cyclone
(marked Filter)
9 Filter pressure outlet
(marked OUT)
11 Heater Inlet
13 Outlet Filter
15 Product collection vessel
17 Connection piece with outlet temperature sensor
19 Spray cylinder
21 On/Off master switch
14 13 12
2 Peristaltic pump 2 (option)
4 Sample and solvent place area
6 Connections on the side
See Chapter 3.2.3 "Connections on the side", page 18
8 Filter pressure inlet
(marked IN)
10 Aspirator outlet
12 Tubing protection (option)
14 Product temperature sensor (option)
16 Cyclone
18 Separation flask
20 Cylinder holder and sensor plugs
See Chapter 3.2.4 "Cylinder holder and sensor plugs", page 18
22 Peristaltic pump 1
Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG
3.2.2
Rear view
13
12
11
10
1 2 3 4
Product description | 3
5
6
7
8
Fig. 3: Rear view
1 Ventilation slots
3 Spray gas
5 Handle
7 Power supply connection
9 Aspirator ventilation
11 Ventilation slots
13 Ventilation slots
9
2 Compressed air for the nozzle cleaner
4 Nozzle
See Chapter 3.2.5 "Spray drying nozzle (Two fluid nozzle)", page 19
6 Spray gas connection
8 Fuses
10 Lower rear door
12 Upper rear door
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3 | Product description
3.2.3
Connections on the side
1 2 3 4 5 6
Büchi Labortechnik AG
Fig. 4: Connections
1 USB
3 USB
5 RJ32
3.2.4
Cylinder holder and sensor plugs
2 USB
4 LAN
6 RJ32
1
2
Fig. 5: Adjustment and sensor plugs
1 Outlet temperature sensor port
3 Product temperature sensor port
2 Handle
3
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3.2.5
Spray drying nozzle (Two fluid nozzle)
1 2 3
Product description | 3
4
3.3
8
7
Fig. 6: Spray drying nozzle
1 Feeding tube connection
(marked FEED)
3 Nozzle needle
5 Dispersion gas connection
(marked GAS)
7 Nozzle tip
6 5
2 Cooling in connection
(marked C IN)
4 Cleaning nozzle gas connection
6 Cooling out connection
(marked C OUT)
8 Nozzle cap
Type plate
The type plate identifies the instrument. The type plate is located at the rear of the instrument.
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3 | Product description Büchi Labortechnik AG
1 2 3
11
10
9
8
7
6
5 4
Fig. 7: Type plate
1 Symbol for "electronics recycling" 2 Initial product code
3 Approvals
5
7
9
Year of manufacture
Frequency
Serial number
11 Company name and address
4 Symbol for "Do not dispose of as household waste"
6 Power consumption maximum
8 Input voltage range
10 Instrument name
3.4
Scope of delivery
NOTE
The scope of delivery depends of the configuration of the purchase order.
Accessories are delivered as per the purchase order, order confirmation, and delivery note.
3.5
Technical data
3.5.1
MiniSprayDryer S-300
MiniSprayDryer
S-300
Dimensions (W x D x H) 620 mm x 640 mm x 1052 mm
Weight (without glass assembly)
54 kg
62.5 kg Weight (with glass assembly)
Connection voltage 220 - 240 ± 10 %
VAC max. 2300 W Power consumption
Fuse
Overvoltage category
Frequency
10 AT
II
50 / 60 Hz
MiniSprayDryer
S-300 Advanced
620 mm x 640 mm x 1052 mm
54 kg
62.5 kg
220 - 240 ± 10 %
VAC max. 2300 W
10 AT
II
50 / 60 Hz
MiniSprayDryer
S-300 Corrosive
620 mm x 640 mm x 1052 mm
54 kg
62.5 kg
220 - 240 ± 10 %
VAC max. 2300 W
10 AT
II
50 / 60 Hz
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Büchi Labortechnik AG Product description | 3
MiniSprayDryer
S-300
IP Code
Pollution degree
IP20
2
100 mm Minimum clearance on all sides
Spray drying gas Nitrogen
Compressed air
Max. pressure spray gas 7 bar
Spray gas range 80-1800 l/min
Max. temperature
Max. flow rate
Sample feed
220 / 250 °C
35 m³/h
0.1-30 ml/min
External connection drying gas
KF25
Certificate CSA / CE
MiniSprayDryer
S-300 Advanced
IP20
2
100 mm
Nitrogen
Compressed air
7 bar
80-1800 l/min
220 / 250 °C
35 m³/h
0.1-30 ml/min
KF25
CSA / CE
MiniSprayDryer
S-300 Corrosive
IP20
2
100 mm
Nitrogen
Compressed air
7 bar
80-1800 l/min
220 / 250 °C
35 m³/h
0.1-30 ml/min
KF25
CSA / CE
3.5.2
Ambient conditions
For indoor use only.
Max. altitude above sea level
Ambient and storage temperature
Maximum relative humidity
2000 m
5 ‒ 40 °C
80% for temperatures up to 31 °C decreasing linearly to 50 % relative humidity at 40 °C
3.5.3
Materials
Component
Housing
Glass assembly
Nozzle
Heater
Product feed tube
Cover of the product collection vessel
Seal of the product collection vessel
Seal cyclone
Drying gas tube
Materials of construction
PUR (Polyurethane) foam painted
3.3 borosilicate glass
Stainless steel
Stainless steel
Silicone and tygon
PA12
FPM
TPR (Thermoplastic elastomers)/PTFE
(Polytetrafluoroethylene)
Acid resistant coated metal
Acid resistant metal
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3 | Product description Büchi Labortechnik AG
3.5.4
Installation site
The installation site meets the safety requirements. See Chapter 2 "Safety", page 9
The installation site has a firm, level and nonslip surface.
The installation site has no obstacles (e.g. water taps, drains, etc.).
The installation site has an own mains outlet socket for the instrument.
The installation site is not exposed to external thermal loads, such as direct solar radiation.
The installation site has enough space that cables / tubes can be routed safely.
The installation site meets the requirements for the connected devices. See related documentation
The installation site meets the specifications according to the technical data (e.g.
weight, dimension, etc.). See Chapter 3.5 "Technical data", page 20
The installation site fits basic electromagnetic environment / Emission Class B.
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4
4.1
Transport and storage | 4
Transport and storage
Transport
NOTICE
Risk of breakage due to incorrect transportation
Make sure that the instrument is fully dismantled.
Pack every instrument components properly to prevent breakage. Use the original packaging whenever possible.
Avoid sharp movements during transit.
4.2
u u u
After transporting, check the instrument and all glass components for damage.
Damage that has occurred in transit should be reported to the carrier.
Keep packaging for future transportation.
Storage
u u u
Make sure that the ambient conditions are complied with (see Chapter 3.5
Wherever possible, store the device in its original packaging.
After storage, check the device, all glass components, seals and tubing for damage and replace if necessary.
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4 | Transport and storage
4.3
Büchi Labortechnik AG
Lifting the instrument
WARNING
Danger due to incorrect transportation
The possible consequences are crushing injuries, cuts and breakages.
u u
Lift the instrument with three persons at the same time.
Lift the instrument at the points indicated.
NOTICE
Dragging the instrument can damage the feet of the instrument.
u
Lift the instrument when positioning or re-locating.
u
Lift the instrument at the points indicated.
2
1 3
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5
5.1
Installation | 5
Installation
Before installation
NOTICE
Instrument damage due to switching it on too early.
Switching on the instrument too early after transportation can cause damage.
u
Climatize the instrument after transportation.
5.2
Establishing electrical connections
NOTICE
Risk of instrument damage because of not suitable power supply cables.
Not suitable power supply cables can cause bad performance or an instrument damage u
Use only BUCHI power supply cables.
5.3
Precondition:
R The electrical installation is as specified on the type plate.
R The electrical installation is equipped with a proper grounding system.
R The electrical installation is equipped with suitable fuses and electrical safety features.
R The installation site is as specified in the
technical date. See Chapter 3.5 "Technical data", page 20
u
Connect the power supply cable to the
connection on the instrument. See Chapter 3.2
u
Connect the mains plug to an own mains outlet socket.
Securing against earthquakes
The instrument has an earthquake fixing point to protect the device against falling.
Operation Manual MiniSprayDryer S-300 25/90
5 | Installation u
Tie the lashing mount to a fixed point using strong cord or a wire.
Büchi Labortechnik AG
5.4
Installing the spray gas supply
Precondition:
R The spray gas supply meets the specifications.
See Chapter 3.5 "Technical data", page 20
u
Attach the air supply to the instrument.
5.5
Installing peristaltic pump 2 (option)
u
Attach the peristaltic pump 2 to the instrument.
u
Connect the cable to the instrument.
26/90
5.6
Installations for remote services (option)
Navigation path:
➔ ➔
Precondition:
R Instrument and mobile device are in the same network.
R The app is installed on the mobile device.
u
Connect the network cable to the socket
marked LAN. See Chapter 3.2 "Configuration", page 15
u
Navigate to the Remote and Monitoring menu according the navigation path.
u
Start the app on the mobile device.
Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG u
Tap the [Scan QR Code] button on the app.
u
Scan the QR code with the app.
ð The mobile device and the instrument are connected.
Installation | 5
5.7
5.8
Installations for a spray drying mode
For installations for a spray drying mode, see separate installation manuals.
"MiniSprayDryer S-300 in closed mode with Dehumidifier and Inert Loop"
"MiniSprayDryer S-300 in closed mode with Inert Loop"
"MiniSprayDryer S-300 in open pressure mode"
"MiniSprayDryer S-300 in open suction mode"
Installing the outlet filter holder
WARNING
Not installed filter holder
A not installed filter holder will result in an inadequately grounded instrument.
A not sufficient grounded instrument can cause fires.
u
Install the filter holder.
u
Put the filter holder onto the instrument.
u
Attach the filter holder to the instrument with the knurl nuts.
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5 | Installation u
Make sure that the warning sign is not visible anymore.
Büchi Labortechnik AG
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6
6.1
Interface
Layout of the interface
1
Interface | 6
3
Fig. 8: Interface
1 Content area
3 Navigation bar
See Chapter 6.2 "Navigation bar", page 29
Using the navigation control
u
Select an entry.
2 Navigation control
2 u
Confirm the selected entry.
6.2
Navigation bar
Icon Description
Menu bar
Home panel
Operation Manual MiniSprayDryer S-300
Further information
Shows available menus.
See Chapter 6.2.1 "Menu bar", page 30
Shows the home screen.
See Chapter 10.4 "Sending instrument data to BUCHI customer service", page 73
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6 | Interface Büchi Labortechnik AG
Icon Description
Methods panel
Job Lists panel
Control panel
Runs panel
Further information
Creating methods
Editing methods
Method library
See Chapter 7.10 "Editing a method (Advanced and Corrosive only)", page 48
Task organization tool.
See Chapter 7.11 "Editing a job list (Advanced and Corrosive only)", page 53
Controlling and editing parameters during a run.
See Chapter 6.2.2 "Control panel", page 30
Shows the details of carried out runs.
See Chapter 8.4 "Exporting run data", page 61
6.2.1
Menu bar
Icon Description
Remote and Monitoring
Settings
Notification
Further Information
See Chapter 5.6 "Installations for remote services (option)", page 26
See Chapter 6.4 "System settings", page 32
See Chapter 6.5 "Customizing options", page 33
Displayed when a notification appears.
Instrument
Logs
Shows details about the spray drying system.
Calibrations
See Chapter 9.2 "Calibrating the peristaltic pumps", page 63
Shows counters and additional information.
Shows the notification history.
Update
Displayed when an update is available.
About
Shows legal information.
6.2.2
Control panel
The control panel consists on three sections:
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Icon Name
Control screen
Description
See Chapter "Control screen", page 31
Live graphs screen Shows live charts of the parameters.
Focus parameters screen Visualizes selected parameters in a larger size.
See Chapter "Customizing the focus parameters screen", page 34
Control screen
Icon Explanation
Solvent
Sample
Stopping the drying gas without stopping the recording of the run.
Auto mode
Function
[Drying gas]
[Inlet T]
[Disper. gas]
[Pump 1]
Description
Set the aspirator flow m 3 /h.
Start the aspirator.
Set of the inlet temperature.
Start heating up the instrument.
Set the spray gas volume in L/h.
Start the gas flow.
Peristaltic pump rate in volume per hour.
Select between detection and flow volume.
Start the spray process.
[Pump 2] (option) Peristaltic pump rate in volume per hour.
Select between detection and flow volume.
[Outlet T]
Start the spray process.
Shows the temperature of the drying gas measured at the end of the drying chamber.
[Product T]
[Deblock]
[Filter press.]
Shows the temperature of the drying gas measured in the product collection vessel.
Setting for the frequency and quantity of the nozzle needle.
Shows the filter permeability in percent or mbar. See Chapter
"Customizing the control screen", page 33
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6 | Interface Büchi Labortechnik AG
6.3
Function buttons
Icon Explanation
[Load] button
[Options] button
[Copy] button
[Delete] button
6.4
System settings
6.4.1
Changing the display settings
The following settings can be changed:
Display setting
[Dark Mode]
[Brightness]
[Dimmer]
Explanation
Uses light texts and icons on a dark background.
Changing the display brightness.
Setting the time the display starts to reduce the brightness.
Navigation path
➔ ➔ [System] u
Navigate to the System submenu according to the navigation path.
u u
Select the Display section.
Carry out the changes according to your needs.
6.4.2
Changing the language settings
Navigation path
➔ ➔ [Customize] u
Navigate to the Customize submenu according to the navigation path.
u u
Select the Localization section.
Select required language from the drop-down menu.
6.4.3
Changing the sound settings
The following sound settings are changeable:
Sound option
[System Volume]
[Keyboard Clicks]
Explanation
Volume setting
Setting the keyboard clicks to ON/OFF
Navigation path
➔ ➔ [System]
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Navigate to the System submenu according to the navigation path.
u u
Select the Sound section.
Carry out the changes according to your needs.
6.4.4
Changing date and time
Options
[Automatic Date and
Time]
[Set Date]
[Select Time Zone]
Explanations
Set the correct time on the instrument automatically
Visible when the [Automatic Data and Time] action is off.
Specify a time offset from local time.
Navigation path
➔ ➔ [System] u
Navigate to the System submenu according to the navigation path.
u u
Select the Date and Time section.
Carry out the changes according to your needs.
6.5
Customizing options
6.5.1
Changing the home screen background
The following graphic formats are possible:
.png
.jpg
Navigation path
➔ ➔ [System]
Precondition:
R A data storage device with graphics is connected to the instrument.
u
Navigate to the System submenu according to the navigation path.
u u
Select the Home Screen section.
Tap the [ + ] button.
ð The display shows the selectable graphics.
u
Select the graphic you wish to enter.
6.5.2
Customize the control panel
Customizing the control screen
The following display options are available:
Display option
Filter Blockage
Filter Pressure
Explanation
Shows the blockage level of the outlet filter in %.
The pressure measured at the outlet of the filter in mbar
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6 | Interface Büchi Labortechnik AG
Navigation path
➔ ➔ [Customize] u
Navigate to the Customize submenu according to the navigation path.
u u
Select the Control Panel section.
Select the filter option you wish to use from the drop-down menu for the [Show
Pressure] action.
Customizing the focus parameters screen
The following options can be selected for each of the three positions:
[Product Temperature]
[Spray Gas]
[Drying Gas]
[Filter Blockage]
[Filter Pressure]
[Outlet Temperature]
[Inlet Temperature]
Navigation path
➔ ➔ [Customize] u
Navigate to the Customize submenu according to the navigation path.
u u
Select the Control Panel section.
Select the option you wish to show from the drop-down menu for each position action.
6.5.3
Customize the report
The following report entries are customizable:
Logo (.jpg or .png only)
Address
Navigation path
➔ ➔ [Customize]
Precondition:
R If necessary, a data storage device with a graphic for the logo is connected to the instrument.
u
Navigate to the Customize submenu according to the navigation path.
u u
Select the Report section.
Tap the [ + ] button.
ð The display shows the selectable graphics.
u
Select the graphic you wish to enter.
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Select the action [Company Address] action.
ð The display shows a dialog with an alphanumeric input box.
u
Enter the address.
ð The entered values are changed.
6.5.4
Changing the measurement units
The following units are changeable:
Type
Temperature
Pressure
Available unit
°C
°F metric imperial
Navigation path
➔ ➔ [Customize] u
Navigate to the Customize submenu according to the navigation path.
u u
Select the Localization section.
Select the measurement units you wish to use.
Interface | 6
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7 Preparing for a spray drying process
7.1
Preparing the outlet filter
7.1.1
Preparing the outlet filter with filter bag (Option)
NOTE
Removing is done in reverse sequence.
u
Put the filter bag on the filter body.
Büchi Labortechnik AG u
Secure the filter bag in place with quick release fastener.
u
Put the prepared filter body in the filter vessel.
u
Secure the filter body in place with the cap nut.
u
Put the filter in the filter holder.
u
Make sure that the filter is attached to the filter holder.
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Connect the filter with the instrument.
Preparing for a spray drying process | 7 u
Attach the filter outlet sensor tube to the filter.
u
Attach the filter inlet sensor tube to the filter.
7.1.2
Preparing the outlet filter with PTFE membrane (Option)
NOTE
Removing is done in reverse sequence.
u
Pull the PTFE membrane on the filter body.
u
Secure the filter bag in place with quick release fastener.
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Turn in the filter membrane.
u
Put the plug on the bottom.
u
Put the prepared filter body in the filter vessel.
u
Secure the filter body in place with the cap nut.
Büchi Labortechnik AG u
Put the filter in the filter holder.
u
Make sure that the filter is attached to the filter holder.
u
Connect the filter with the instrument.
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Attach the filter outlet sensor tube to the filter.
Preparing for a spray drying process | 7 u
Attach the filter inlet sensor tube to the filter.
7.2
Preparing the glass assembly
NOTE
Removing is done in reverse sequence.
Precondition:
R
The filter is prepared. See Chapter 7.1
"Preparing the outlet filter", page 36
u
Open the handle at the adjustment.
u
Attach the seal holder with the seal onto the instrument.
u
Attach the separation flask to the spray cylinder.
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Attach the coupling flange to the spray cylinder.
Büchi Labortechnik AG u
Open the handle.
u
Press the prepared spray cylinder on the seal holder.
u
Make sure, that the connection for the outlet sensor shows in the direction indicated.
u
Turn the spray cylinder that the coupling flange fits the adjustment.
u
Close the handle.
u
Fix the handle at the adjustment.
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Precondition:
R The product collection vessel is prepared. See
Chapter 7.3 "Preparing the product vessel", page 41
u
Attach the cyclone to the spray cylinder.
Preparing for a spray drying process | 7 u
Attach the cyclone to the filter.
7.3
Preparing the product vessel
NOTE
Removing is done in reverse sequence.
u
Prepare the product collection vessel.
u
Attach the prepared product vessel to the cyclone.
7.4
Preparing the spray drying nozzle
Attaching and removing hoses to the nozzle:
Operation Manual MiniSprayDryer S-300 41/90
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Press the ring at the connector.
u
Move the hose.
Precondition:
R The peristaltic pump is prepared. See
Chapter 7.5 "Preparing the peristaltic pump", page 43
u
Insert the nozzle into the heater element of the spray dryer.
u
Attach the spray gas onto the connection marked GAS.
u
Attach the inlet tube in place with the union nut.
Büchi Labortechnik AG u
Attach the compressed gas to the nozzle.
u
Attach the assembled feeding tube onto the connection marked FEED.
u
Attach the inlet tube in place with the union nut.
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7.5
Preparing the peristaltic pump
7.5.1
Preparing the peristaltic pump for manual mode
Precondition:
R The peristaltic pump bed is prepared. See
Chapter 7.8 "Adjusting the peristaltic pump bed", page 46
R The solvent is prepared.
R Sample is prepared.
u
Prepare the feeding tube.
u
Lower the hose base.
u
Install the feeding tube.
u
Close the hose base.
7.5.2
Preparing the peristaltic pump for auto mode (option)
Precondition:
R The peristaltic pump bed is prepared. See
Chapter 7.8 "Adjusting the peristaltic pump bed", page 46
R The solvent is prepared.
R Sample is prepared.
u
Prepare the Y-piece.
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Lower the hose base.
u
Attach the tube with the sample in the rear guide.
u
Attach the tube with the solvent in the front guide.
u
Close the hose base.
Büchi Labortechnik AG u
Connect the feeding tube to the nozzle. See
Chapter 7.4 "Preparing the spray drying nozzle", page 41
7.6
Preparing the sensors
7.6.1
Preparing the product temperature sensor (option)
(first time only) u
Remove the cap nut from the product collection vessel.
(first time only) u
Remove the sealing from the cap nut.
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(first time only) u
Attach the sealing to the sensor.
Preparing for a spray drying process | 7 u
Attach the cap nut to the sensor.
u
Attach the sensor to the product collection vessel.
u
Connect the sensor to the instrument.
7.6.2
Preparing the outlet temperature sensor
(first time only) u
Remove the cap nut from the sensor mounting.
(first time only) u
Remove the sealing from the cap nut.
(first time only) u
Attach the sealing to the sensor.
Operation Manual MiniSprayDryer S-300 45/90
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Attach the cap nut to the sensor.
u
Attach the sensor to the sensor mounting.
u
Connect the sensor to the instrument.
Büchi Labortechnik AG
7.7
Preparing the grounding (if no product sensor is used)
u
Attach the grounding cable to the product collection vessel.
u
Connect the grounding cable to the instrument.
7.8
Adjusting the peristaltic pump bed
Tools needed:
Torx size 15
Order no.
none
Image
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Navigation path
➔ u
Select a suitable feeding tube. See
Chapter 12.1.1 "Feeding tube", page 75.
u
Prepare the solvent.
u
Lower the hose base.
Preparing for a spray drying process | 7 u
Install the feeding tube.
u
Put the other end of the tube in a n beaker flask.
u
Close the hose base.
7.9
u
Navigate to the Control panel according the navigation path.
u
Tab the Start peristaltic pump button.
u
Close the pump bed that no liquid can pass.
u
Turn the key 1/4 the opposite side.
u
Calibrate the peristaltic pump. See Chapter 9.2
"Calibrating the peristaltic pumps", page 63
Preparing the instrument for remote services (option)
NOTE
Press the [Take Back Control] button on the display to interrupt the connection to the mobile device.
There are two remote services available:
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Remote type
[Remote Control]
Explanation
Carrying out the instrument functions from an remote device.
Monitoring all values from an remote device.
[Monitoring]
Navigation path:
➔ ➔
Precondition:
R
The instrument and the mobile device are prepared. See Chapter 5.6
"Installations for remote services (option)", page 26
u u
Tap the [Start Remote] button on the instrument.
Select the remote service on the app.
ð The instrument and the app are connected.
7.10
Editing a method (Advanced and Corrosive only)
7.10.1 Creating a new method
NOTE
It is not possible to enter a name twice.
Creating a new method
Navigation path
➔ u u u
Navigate to the Methods menu according to the navigation path.
Tap the [ + ] button.
Select the [Name] action.
ð The display shows a dialog with an alphanumeric input box.
u u
Enter a name for the method.
Tap the [Save] button.
ð The method is created.
Creating a new method by copying an existing
Navigation path
➔ u u u u u
Navigate to the Methods menu according to the navigation path.
Tap the [Options] button.
Tap the [Duplicate] action.
Select the method you wish to copy.
Tap the [Duplicate] button.
ð The copy is created.
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7.10.2 Deleting a method
Navigation path
➔ u u u u u
Navigate to the Methods menu according to the navigation path.
Tap the [Options] button.
Tap the [Delete] action.
Select the method you wish to delete.
Tap the [Delete] button.
ð The method is deleted.
7.10.3 Changing the name of a method
Navigation path
➔
Precondition:
R The method is not loaded.
u u u u
Navigate to the Methods menu according to the navigation path.
Select the method you wish to edit.
Select the Basic Information section.
Select the action [Name].
ð The display shows a dialog with an alphanumeric input box.
u u
Enter a name for the method.
Tab the [Save] button.
ð The method name is changed.
7.10.4 Changing the description for a method
Navigation path
➔
Precondition:
R The method is not loaded.
u u u u
Navigate to the Methods menu according to the navigation path.
Select the method you wish to edit.
Select the Basic Information section.
Select the [Description] action.
ð The display shows a dialog with an alphanumeric input box.
u u
Enter a description for the method.
Tab the [Save] button.
ð The description for the method is saved.
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7.10.5 Changing the drying gas volume for a method
Navigation path
➔
Precondition:
R The method is not loaded.
u u u u
Navigate to the Methods menu according to the navigation path.
Select the method you wish to edit.
Select the Method Parameters section.
Select the [Drying Gas] action.
ð The display shows a dialog box with a numeric input box.
u u
Enter the drying gas volume in m³/h.
Tab the [Save] button.
ð The drying gas volume is saved.
7.10.6 Changing the inlet temperature for a method
Navigation path
➔
Precondition:
R The method is not loaded.
u u u
Navigate to the Methods menu according to the navigation path.
Select the method you wish to edit.
Select the Method Parameters section.
ð The display shows a dialog box with a numeric input box.
u u u
Select the [Inlet Temperature] action.
Enter the target value in °C.
Tab the [Save] button.
ð The inlet temperature is saved.
7.10.7 Changing the dispersion gas volume for a method
Navigation path
➔ u u
Navigate to the Methods menu according to the navigation path.
Select the method you wish to edit.
u u u
Select the Method Parameters section.
Select the [Dispersion Gas] action.
Enter the target dispersion gas volume L/h.
ð The display shows a dialog box with a numeric input box.
u
Tab the [Save] button.
ð The dispersion gas volume is saved.
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7.10.8 Changing the pump volume for a method
Navigation path
➔ u u u
Navigate to the Methods menu according to the navigation path.
Select the method you wish to edit.
Select the Method Parameters section.
ð The display shows a dialog box with a numeric input box.
u u u
Select the [Pump] action.
Enter the pump volume in mL/min.
Tab the [Save] button.
ð The pump volume is saved.
7.10.9 Changing the outlet temperature for a method
This action sets the alarm value for the outlet temperature.
The instrument does not carry out any additional actions.
Navigation path
➔
7.10.1
0
u u u u
Navigate to the Methods menu according to the navigation path.
Select the method you wish to edit.
Select the Method parameters section.
Select the [Outlet Temp. Alarm] action.
ð The display shows a dialog box with a numeric input box.
u u
Enter the outlet temperature in °C.
Tab the [Save] button.
ð The outlet temperature is saved.
Changing the product temperature for a method
This action sets the alarm value for the product temperature.
The instrument does not carry out any additional actions.
Navigation path
➔ u u
Navigate to the Methods menu according to the navigation path.
Select the method you wish to edit.
u u
Select the Method parameters section.
Select the [Product Temp. Alarm] action.
ð The display shows a dialog box with a numeric input box.
u u
Enter the product temperature in °C.
Tab the [Save] button.
ð The product temperature is saved.
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7.10.1
1
Changing the nozzle deblock frequency for method
Navigation path
➔
7.10.1
2
u u
Navigate to the Methods menu according to the navigation path.
Select the method you wish to edit.
u u
Select the Method parameters section.
Select the [Deblock Nozzle] action.
ð The display shows a dialog box with a numeric input box.
u u
Enter the deblock speed in bpm.
Tab the [Save] button.
ð The deblock speed of the nozzle is saved.
Importing a method
the following method format is possible:
.bdmf
Navigation path
➔
7.10.1
3
Precondition:
R A data storage device with a method is connected to the instrument.
u u u u
Navigate to the Methods menu according to the navigation path.
Tap the [Options] button.
Tap the [Import] action.
Select the method you wish to import.
ð A dialog confirms the method import.
Exporting a method
Navigation path
➔
Precondition:
R A data storage device is connected to the instrument.
u u u u u u
Navigate to the Methods menu according to the navigation path.
Tap the [Options] button.
Select the [Export] action.
Select the method you wish to export.
Tap the [Export] button.
Select the export folder.
ð A message confirms the method export.
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7.10.1
4
Loading a method
Navigation path
➔
Precondition:
R
A method is created. See Chapter 7.10 "Editing a method (Advanced and
u u
Navigate to the Methods menu according to the navigation path.
Tap the load method button for the method you wish to use.
ð The method is loaded.
7.11
Editing a job list (Advanced and Corrosive only)
NOTE
It is not possible to enter a name twice.
7.11.1 Creating a new job list
Navigation path
➔ u u u
Navigate to the Job Lists panel.
Tap the [ + ] button.
Select the [Name] action.
ð The display shows a dialog with an alphanumeric input box.
u u u
Select a method for the job list.
Enter a name for the job list entry.
Tap the [Save] button.
ð The job list is created.
7.11.2 Adding an entry to a job list
Adding an entry to a job list
Navigation path
➔ u u u
Navigate to the Job Lists panel.
Select the job list which you want to add an entry.
Tap the [ + ] button.
ð The display shows a dialog with an alphanumeric input box.
u u u u
Enter a name for the job list entry.
Select a method for the job list entry.
Enter a description for the entry.
Tap the [Save] button.
ð The job list is created.
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Adding an entry to a job list by copy an existing
Navigation path
➔ u u u u u
Navigate to the Job Lists panel.
Select the job list which you want to add an entry.
Select the job list entry you wish to copy.
Tap the [Copy] button.
Tap the [Save] button.
ð A message confirms the job list entry.
7.11.3 Deleting a job list
Navigation path
➔ u u u u u
Navigate to the Job Lists panel.
Tap the [Options] button.
Tap the [Delete] action.
Select the job list you wish to delete.
Tap the [Delete] button.
ð The job list is deleted.
7.11.4 Deleting a job list entry
Navigation path
➔ u u u u u
Navigate to the Job Lists panel.
Select the job list in which you want to delete an entry.
Select the job list entry you wish to delete.
Tap the [Delete] button.
Tap the [Save] button.
ð A message confirms the job list entry.
7.11.5 Loading a job list
Navigation path
➔
Precondition:
R
A job list is created. See Chapter 7.11 "Editing a job list (Advanced and Corrosive only)", page 53
u u
Navigate to the Job Lists panel.
Tap the load button for the job list you wish to use.
ð The job list is loaded.
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7.12
Editing an auto mode sequence (Advanced and Corrosive only)
The following functions are programable:
Function Description
[Pump 1] Select between detection and flow volume.
[Remaining Volume of Solvent]
[Remaining Volume of Sample]
Start the spray process.
Enter the volume of pure solvent to be transported before switching to the sample.
Enter the volume of sample to be transported before switching back to the pure solvent.
[Auto Mode State] Select a spray drying phase. Selection possibilities depends on the instrument status.
➔ ➔ u u u u
Navigate to the Auto sequence action according the navigation path.
Enter the requested values.
Select the [Auto Mode State] you wish to use.
Tap the [Start] button.
ð The instrument starts a spray drying process with the set parameters.
7.13
Tagging table entries
A tag is keyword assigned to a table entry. This helps to describe an entry better and allows it to be found again by browsing or searching.
u
Select the table entry you wish to tag.
u u u
Select the Basic Information section.
Select the [Tags] action.
Tap the [ + ] button.
ð The display shows a dialog with an alphanumeric input box.
u u
Enter a name for the tag.
Tab the [Save] button.
ð The list entry is tagged.
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8
8.1
Carrying out a spray drying process
NOTE
To minimizing negative environmental affects during operation: u
Follow the instructions in the corresponding "Application Note".
Preparing the instrument for monitoring
Navigation path:
➔ ➔
Precondition:
R
The instrument and the mobile device are prepared. See Chapter 5.6
"Installations for remote services (option)", page 26
u
Tap the [Monitor] button on the app.
8.2
Carrying out a spray drying process in open mode
8.2.1
Preparing the instrument for open mode
Precondition:
R
All commissioning operations have been completed. See Chapter 5 "Installation", page 25
R A configuration for the open mode is installed. See related "Installation Manual" u
Set the On/Off master switch to on.
ð The instrument is starting up.
u u u u u u u u
Prepare the pure solvent.
Prepare the sample.
Place sample and solvent on the sample place area.
Prepare the peristaltic pump. See Chapter 7.5 "Preparing the peristaltic pump", page 43
Prepare the spray drying nozzle. See Chapter 7.4 "Preparing the spray drying nozzle", page 41
Make sure that the tubing is not bend.
Make sure that no defective sealings or glass parts are used.
Prepare the glass assembly. See Chapter 7.2 "Preparing the glass assembly", page 39
8.2.2
Starting a spray drying process in open mode
Start the spray drying process according to your needs:
Chapter "Starting a spray drying process in open mode manually", page 57
Chapter "Starting a spray drying process in open auto mode (Advanced and
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Starting a spray drying process in open mode manually
NOTE u
There are three possibilities to carry out the manual mode:
ð Carrying out each parameter individually.
ð
With a method. See Chapter 7.10 "Editing a method (Advanced and Corrosive only)", page 48
ð
With a job list. See Chapter 7.11 "Editing a job list (Advanced and Corrosive only)", page 53
Navigation path
➔
Precondition:
R
The instrument is prepared. See Chapter 8.2.1 "Preparing the instrument for open mode", page 56
u u u
If necessary, load a method. See Chapter 7.10.14 "Loading a method", page 53
If necessary, load a job list. See Chapter 7.11.5 "Loading a job list", page 54
Navigate to the Control panel according the navigation path.
u u
If necessary, adjust the drying gas volume.
Tap the drying gas start button.
ð The aspirator is starting up.
u u u u
If necessary, adjust the spray gas volume.
Tap the spray gas start button.
If necessary, adjust the inlet temperature.
Tap the inlet temperature start button.
ð The instrument is heating up.
u u u u
Wait until the system is in steady conditions.
Immerse the tube in the solvent.
If necessary, adjust the peristaltic pump volume.
Tap the peristaltic pump start button.
ð The solvent flows to the nozzle.
Starting a spray drying process in open auto mode (Advanced and Corrosive only)
NOTE u
There are three possibilities to carry out the auto mode:
ð
ð
With a method. See Chapter 7.10 "Editing a method (Advanced and Corrosive only)", page 48
ð
With a job list. See Chapter 7.11 "Editing a job list (Advanced and Corrosive only)", page 53
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Navigation path
➔
Precondition:
R
The instrument is prepared. See Chapter 8.2.1 "Preparing the instrument for open mode", page 56
u u u u u
If necessary, load a method. See Chapter 7.10.14 "Loading a method", page 53
If necessary, load a job list. See Chapter 7.11.5 "Loading a job list", page 54
Navigate to the Control panel according the navigation path.
Tap the drying gas start button.
ð The instrument starts the auto mode.
8.2.3
Tasks during spray drying (manual mode only)
Precondition:
R
u
Change the feed tube from the pure solvent to the sample.
ð The sample flows though the feed tube to the nozzle.
8.2.4
Ending a spray drying process in open mode
Precondition:
R The sample beaker is empty.
u u
Change the feed tube from the sample to the solvent.
Wait 2 -3 minutes.
ð The solvent flushes the remains from the nozzle.
u u u u u u u u u
Remove the sample tube from the solvent vessel.
Wait until the tube is empty.
Tap the peristaltic pump stop button.
Tap the spray gas stop button.
Tap the heater stop button.
If necessary save the run.
Wait until the glassware is in ambient temperature.
Tap the aspirator stop button.
Remove the product from the product collection vessel.
8.2.5
Shutting down the instrument
Precondition:
R
u u
Switch the On/Off master switch to Off.
Clean the nozzle. See Chapter 9.10 "Cleaning the nozzle", page 67.
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8.3
Carrying out a spray drying process in closed mode
There are two different modes closed mode:
Closed mode with inert loop
Closed mode with inert loop and dehumidifier
8.3.1
Preparing the instrument for closed mode
Low drying temperature ca. 80 °C approx. 15 min
High drying temperature ca. 220 °C approx. 30 min Time required:
Precondition:
R
All commissioning operations have been completed. See Chapter 5 "Installation", page 25
R A configuration for the closed mode is installed. See related "Installation Manual" u
Set the On/Off master switch to On.
ð The instrument is starting up.
u u u u u u u u
Prepare pure solvent.
Prepare the sample.
Place sample and solvent on the sample place area.
Prepare the peristaltic pump. See Chapter 7.5 "Preparing the peristaltic pump", page 43
Prepare the spray drying nozzle. See Chapter 7.4 "Preparing the spray drying nozzle", page 41
Make sure that no defective sealings or glass parts are used.
Make sure that the tubing is not bend.
Prepare the glass assembly. See Chapter 7.2 "Preparing the glass assembly", page 39
8.3.2
Starting a spray drying process in closed mode
Starting a spray drying process in closed auto mode (Advanced and
Corrosive only)
NOTE u
There are three possibilities to carry out the auto mode:
ð
ð
With a method. See Chapter 7.10 "Editing a method (Advanced and Corrosive only)", page 48
ð
With a job list. See Chapter 7.11 "Editing a job list (Advanced and Corrosive only)", page 53
Navigation path
➔
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Precondition:
R
The instrument is prepared. See Chapter 8.3.1 "Preparing the instrument for closed mode", page 59
u u u u u u u
Select the condenser temperature at the Inert Loop.
For closed mode with inert loop and dehumidifier set the On/Off master switch of the dehumidifier to on.
If necessary, load a method. See Chapter 7.10.14 "Loading a method", page 53
If necessary, load a job list. See Chapter 7.11.5 "Loading a job list", page 54
Navigate to the Control panel according the navigation path.
Tap the drying gas start button.
ð The instrument starts the auto mode.
Starting a spray drying process in closed mode manually
NOTE u
There are three possibilities to carry out the manual mode:
ð Carrying out each parameter individually.
ð
With a method. See Chapter 7.10 "Editing a method (Advanced and Corrosive only)", page 48
ð
With a job list. See Chapter 7.11 "Editing a job list (Advanced and Corrosive only)", page 53
Navigation path
➔
Precondition:
R
The instrument is prepared. See Chapter 8.3.1 "Preparing the instrument for closed mode", page 59
u u u u
Select the condenser temperature at the Inert Loop.
For closed mode with inert loop and dehumidifier set the On/Off master switch of the dehumidifier to On.
If necessary, load a method. See Chapter 7.10.14 "Loading a method", page 53
If necessary, load a job list. See Chapter 7.11.5 "Loading a job list", page 54
u u u
Navigate to the Control panel according the navigation path.
If necessary, adjust the drying gas volume.
Tap the drying gas start button.
ð The aspirator is starting up.
ð The oxygen level decreases.
ð The spray gas starts.
u u u
Wait until the oxygen level is less than 6%.
If necessary, adjust the inlet temperature.
Tap the inlet temperature start button.
ð The instrument is heating up.
u
Wait until the system is in steady conditions.
60/90 Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG Carrying out a spray drying process | 8 u u u
Immerse the tube in the solvent.
If necessary, adjust the peristaltic pump volume.
Tap the peristaltic pump start button.
ð The solvent flows to the nozzle.
8.3.3
Tasks during spray drying (manual mode only)
Precondition:
R
u
Change the feed tube from the pure solvent to the sample.
ð The sample flows though the feed tube to the nozzle.
8.3.4
Ending a spray drying process in closed mode
Precondition:
R The sample beaker is empty.
u u u
Change the feed tube from the sample to the pure solvent.
Decrease the pump rate.
Wait 2 -3 minutes.
ð The solvent flushes the remains from the nozzle.
u u u u u u u u u
Remove the sample tube from the solvent vessel.
Wait until the tube is empty.
Tap the peristaltic pump stop button.
Tap the heater stop button.
If necessary save the run.
Wait until the glassware is in ambient temperature.
Tap the aspirator stop button.
Set the air flow to 0.
Remove the product from the product collection vessel.
8.3.5
Shutting down the instrument
Precondition:
R
u u u
Switch the On/Off master switch to Off.
For closed mode with inert loop and dehumidifier set the On/Off master switch of the dehumidifier to Off.
Clean the nozzle. See Cleaning and servicing
8.4
Exporting run data
.csv
Navigation path
➔
Operation Manual MiniSprayDryer S-300 61/90
8 | Carrying out a spray drying process
8.5
8.6
Precondition:
R A data storage device is connected to the instrument.
u u u u u u
Navigate to the Runs panel according the navigation path.
Tap the [Options] button.
Select the export format you wish to use.
Select the run you wish to export.
Tap the [Export] button.
Select the export folder.
ð A message confirms the run export.
Deleting run data
Navigation path
➔ u u u u u
Navigate to the Runs panel according the navigation path.
Tap the [Options] button.
Tap the [Delete] action.
Select the run you wish to delete.
Tap the [Delete] button.
ð The run is deleted.
Disconnecting the remote services
Precondition:
R The display shows the [Take Back Control] button.
u
Tap the [Take Back Control] button.
Büchi Labortechnik AG
62/90 Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG
9
9.1
Cleaning and servicing | 9
Cleaning and servicing
NOTE u u u u
Carry out only the service and cleaning operations described in this section.
Do not carry out any servicing and cleaning operations that involve opening the housing.
Use only genuine BUCHI spare parts in order to ensure correct operation and preserve the warranty.
Carry out the service and cleaning operations described in this section to extant the lifetime of the instrument.
Regular maintenance work
9.2
Action
Calibrating the peristaltic pumps
1
1
1
1
Weekly Additional information
Calibrate the peristaltic pumps before every use.
Carry out this action after every instrument use.
Clean the spray drying nozzle after every use.
Cleaning and servicing the drying gas hoses
Cleaning and servicing the warning and directive symbols
1 - User; 2 - Operator
Calibrating the peristaltic pumps
Navigation path
➔ ➔ ➔
1
2
2
2 u u u
Precondition:
R
The peristaltic pump is prepared. Chapter 7.5 "Preparing the peristaltic pump", page 43
R A measuring cylinder is available.
R A calibration sample with the same viscosity as the sample is available.
Fill the tube with the calibration sample.
Put the sample feeding tube in the calibration sample.
Put the other end in the measuring cylinder.
Operation Manual MiniSprayDryer S-300 63/90
9 | Cleaning and servicing
9.3
9.4
Büchi Labortechnik AG u u u u u u u
Navigate to the Maintenance submenu via the navigation path.
Remove the air bubbles.
Enter the necessary calibration volume.
Enter the necessary calibration time.
Tap the [Start Calibration] button.
Wait until the calibration time is over.
Enter the difference between target value and actual value.
Cleaning the aspirator
NOTE
Do not immerse the tube into the water.
Be aware that no splashes are contaminating the ambient at the outlet side.
Navigation path
➔ u u u u u u u u u u u
Fill a vessel with 2L water.
Prepare an empty canister with a small opening.
Insert the exhaust tube from the aspirator into one third of the empty canister.
Remove the spray gas supply.
Fix the tube.
Set the aspirator to 20 m 3 /h.
Set the aspirator to on.
Carefully move the inlet tube over the surface of the water to suck in a mixture of air and water.
Increase the aspirator rate up to 28 m 3 /h.
Continue this procedure unless clean water is coming out of the aspirator.
Wait until the aspirator is dry.
u u u
Navigate to the Control panel according the navigation path.
Set the drying gas to the necessary volume.
Tap the drying gas start button.
ð The aspirator is starting up.
u
Wait until the aspirator is dry.
Opening and closing the lower rear door.
u
Push the snap lock down and pull the door.
64/90 Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG u
Remove the exhaust air hose.
u
Remove the door.
Cleaning and servicing | 9
9.5
Opening and closing the upper rear door
u
Push the snap lock down and pull the door.
u
Remove the door.
9.6
Cleaning and servicing the drying gas hoses
Navigation path
➔ u
Check the hoses for degradation.
ð If necessary replace them.
u u u
Remove all hoses from the instrument.
Rinse the hoses with water.
Install the hoses according the related installation manual.
u u u
Navigate to the Control panel according the navigation path.
Set the drying gas to the necessary volume.
Tap the drying gas start button.
ð The aspirator is starting up.
u u
Wait until the hoses are dry.
Tap the stop button.
Operation Manual MiniSprayDryer S-300 65/90
9 | Cleaning and servicing
9.7
9.8
Büchi Labortechnik AG
Cleaning the filter
u u
Check if the outlet filter pressure is not more than 20 mbar relative to the clean filter.
If necessary, clean or replace the filter. See Chapter 7.1 "Preparing the outlet filter", page 36
Cleaning the heater
NOTE
Installing is done in reverse sequence.
Precondition:
R The instrument is not connected to the electric grid.
u
Wait until the heater is in ambient temperature.
u
Open the upper rear door. See Chapter 9.5
"Opening and closing the upper rear door", page 65
u
Disconnect the plug.
u
Open the screw from the heater.
u
Remove the heating element.
u
Brush the heating element.
66/90
9.9
Cleaning the glass component
u
Check the glass ware for mechanical defects.
ð If necessary, replace them.
u u
Check the glass ware for residues.
Check the glass wall of the main body and the connectors.
ð If the part is dirty, clean it with detergents.
ð If the glass part is showing deterioration or leakages, replace it.
Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG
9.10
Cleaning the nozzle
NOTICE
Sharp cleaning tools
Sharp cleaning tools can damage the surface.
u
Do not use any sharp cleaning tools.
Cleaning and servicing | 9
NOTICE
Liquids in cooling gas channels.
Liquids in cooling gas channels cause damage.
u
Make sure that no liquids get into the cooling gas channels during the cleaning process.
u
Remove the cleaning head.
u
Remove the nozzle cap.
u
Remove the nozzle tip.
Operation Manual MiniSprayDryer S-300 67/90
9 | Cleaning and servicing u
Clean the nozzle with a small cleaning brush, cleaning agent and water.
Büchi Labortechnik AG u
Clean the with a damp cloth, leaning agent and water.
9.11
Cleaning and servicing the warning and directive symbols
u u
Check that the warning symbols on the instrument are legible.
If they are dirty, clean them.
9.12
Cleaning the housing
u u u
Wipe down the housing with a damp cloth.
If heavily soiled, use ethanol or a mild detergent.
Wipe down the display with a damp cloth.
68/90 Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG Help with faults | 10
10 Help with faults
10.1
Troubleshooting
10.1.1 Troubleshooting general
Problem Possible cause Action
Instrument cannot be switched on.
Peristaltic pump does not apply solvent.
Product drips in spray chamber.
No electric connection.
u
Establish an electrical
"Establishing electrical connections", page 25
The rollers are not in contact with the running surface.
u
Lift the hose base.
u
Adjust the peristaltic pump
"Adjusting the peristaltic pump bed", page 46
Product is delivered after the spray flow is switched on although the pump is switched off.
Nozzle is block.
Feed tube defective.
u
Replace the feed tube.
The pressure of the rollers on the running surface is too weak.
u
Adjust the peristaltic pump
"Adjusting the peristaltic pump bed", page 46
Product is too concentrated.
u
Use a lower concentration in pump.
Encrustation on nozzle exit.
u
Clean the nozzle. See
Chapter 9.10 "Cleaning the nozzle", page 67
Nozzle is defective (e.g. bent nozzle needle).
u
Replace nozzle or defective part.
Irregular or pulsed spraying.
Leaks in the spray nozzle.
u
Check seals in the spray nozzle.
u
If necessary, replace the seals.
No spray flow.
Insufficient spray flow.
u
Open spray gas valve.
u
Check pressure of the spray gas in the supply tube (5–8 bar).
Operation Manual MiniSprayDryer S-300 69/90
10 | Help with faults Büchi Labortechnik AG
Problem
Deposits on the spray cylinder.
Glass elements become wet.
Deposits in the cyclone.
Possible cause Action
Nozzle is not clean.
Nozzle is defective (bent nozzle needle).
Product will not dry.
u
Clean the nozzle. See
Chapter 9.10 "Cleaning the nozzle", page 67
u
Replace nozzle or defective part.
u
Reduce the temperature difference between entry and exit u
Increase rate of gas spray flow
(> 600 l/h) u
Reduce peristaltic pump performance.
Entry temperature is above the melting point of the product.
u
Reduce entry temperature.
Product related deposits.
No action possible.
Wide spray angle deposits droplet on the spray cylinder wall.
u
Narrow the spray angle by adjusting the spray cap position.
Peristaltic pump lever has become loose.
u
Tighten lever.
Product related deposits.
No measure possible.
Static charge build-up.
u
Check gas supply pressure.
Product too moist.
Temperature too high.
u
Check tube condition.
u
Insert earthing cable.
u
Increase exit temperature to dry the product.
u
Reduce aspirator performance to reduce residence time of product.
70/90 Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG Help with faults | 10
10.1.2 Troubleshooting heater
Problem
System does not heat up.
Exit temperature does not rise.
Entry temperature falls.
Exit temperature falls.
Exit temperature rises
Possible cause
The heater is not connected properly.
Nominal entry temperature is below room temperature.
Fuse has blown
Action u
Check the heater plug.
u
Pre-select a new inlet temperature.
u
Change the fuse. See
Chapter 10.3 "Changing the fuse", page 72
u Contact BUCHI Customer
Service.
Heater defective
Faulty tubing system
(Faulty flow direction or no flow in the heating system)
Sensor not inserted.
Fault in tubing system.
u
Replace the heater.
u
Check tubing system.
u Contact BUCHI Customer
Service.
Heating is switched off.
Fuse has blown.
Spraying too powerful
Nozzle blocked u
Place probe in coupling element.
u
Check tubing system.
u
Switch on heating.
u
Change the fuse. See
Chapter 10.3 "Changing the fuse", page 72
u
Reduce production rate of peristaltic pump.
u
Clean the nozzle by actuating the cleaning button or by switching on cleaning nozzle.
u
Increase number of pulses for the nozzle cleaning activity.
Hose not dipped into stock solution Change of concentration in stock solution
No feed of product u
Dip hose into product.
u
Agitate product (magnetic agitator)to obtain uniform concentration.
u
Switch on peristaltic pump
Operation Manual MiniSprayDryer S-300 71/90
10 | Help with faults Büchi Labortechnik AG
10.1.3 Troubleshooting aspirator
Problem
Aspirator is noisy.
Insufficient aspirator performance.
Possible cause
The aspirator is dirty.
Action u
Clean the aspirator. See
Chapter 9.3 "Cleaning the aspirator", page 64
The operating mode is set to blow u
If no discharge filter is fitted, this should be done to avoid further contamination of the aspirator.
u
Reset to suction mode if possible.
Discharge filter blocked.
u
Dismantle filter and clean it.
10.2
Nozzle does not atomize
u u
Check if all electrical connections are properly installed.
Check the nozzle power setting on the controller.
ð Make sure that a sufficient setting is used.
u u
Check the peristaltic pump is working properly.
Check all connections of the liquid feeding line.
ð Insufficient liquid supply can cause a high temperature to build up on the nozzle.
10.3
Changing the fuse
WARNING
Risk of electric shock with connected power supply cable.
Serious injuries or death can result.
u u
Switch off the device.
Disconnect the power supply cable from the device.
u u u
Set the On/Off master switch to Off.
Disconnect the power supply cable from the device.
Unscrew the fuse carrier (2).
ð Make sure the O-ring on the fuse carrier is not damaged.
u u u
Replace the defective fuse (1).
Screw in the fuse carrier.
Connect the power supply cable.
72/90 Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG Help with faults | 10 u
If the fuse brakes repeatedly contact the Contact BUCHI Customer Service .
10.4
Sending instrument data to BUCHI customer service
Navigation path
➔
Precondition:
R A data storage device is connected to the instrument.
u u u u
Navigate to the Home menu according the navigation path.
Tap the [Support] button.
Save the data on the storage device.
Send the data to BUCHI customer service.
10.5
No liquid delivery
u
Check the condition of the tube used in the peristaltic pump.
ð Replace a worn out tube.
u
Adjust the peristaltic pump bed. See Chapter 7.8 "Adjusting the peristaltic pump bed", page 46
Operation Manual MiniSprayDryer S-300 73/90
11 | Taking out of service and disposal Büchi Labortechnik AG
11 Taking out of service and disposal
11.1
Taking out of service
u u u u
Remove all solvents and coolants.
Clean the instrument.
Switch off the instrument and disconnect it from the mains power supply.
Remove all tubing and communication cables from the device.
11.2
Disposal
The operator is responsible for proper disposal of the instrument.
u
When disposing of equipment observe the local regulations and statutory u requirements regarding waste disposal.
When disposing, observe the disposal regulations of the materials used. Materials
used see Chapter 3.5 "Technical data", page 20
11.3
Returning the instrument
Before returning the instrument, contact the BÜCHI Labortechnik AG Service
Department.
https://www.buchi.com/contact
74/90 Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG Appendix | 12
12 Appendix
12.1
Material information
12.1.1 Feeding tube
Solvent
Methanol
Ethanol
Acetone
Toluene
Isopropanol
Chloroform
Dichloromethane
Tetrahydrofuran
Ethylacetate
Hexane
Acetonitrile (ACN)
12.1.2 Drying gas hoses
Medium
Chloroform
Dichloromethane
Methanol
Ethanol
Acetone
Toluene
Acetonitrile
Tetrahydrofuran
Ethyl acetate
Hexane
Hydrochloric acid
Sulfuric acid
Acetic acid
Formic acid
Sodium hydroxide
Ammonia
Water
Concentration
%
100
100
100
100
100
100
100
100
100
96
100
50
70
100
100
100
Silicone tube Tygon MH 2375 Tygon F 4040 A
-
-
+
+
-
-
+
-
-
-
-
-
-
-
-
+
+
+
+
+
-
-
-
-
-
-
+
+
+
+
Resistance
+
+
+
+
+
+
+
+
+
+
/
/
+
/
+
Operation Manual MiniSprayDryer S-300 75/90
12 | Appendix
12.2
Spare parts and accessories
12.2.1 Nozzle
Three-fluid nozzle, complete
Nozzle for two independent sample feeds at the same time.
Allows to spray dry immiscible samples for microencapsulation applications.
Two-fluid nozzle corrosives, complete
Order no.
046555
11056320
Büchi Labortechnik AG
Image
Three-fluid nozzle corrosives, complete
Two-fluid nozzle 0.7 mm, complete
11056971
044698
Three-fluid nozzle conversion kit
Nozzle cleaning 0.7 mm, complete
046556
044643
Cleaning brush for nozzle 044782
O-ring for nozzle cleaner, FKM (black), 2× 044469
Nozzle exchange set 1.4 mm, complete
Wider diameter for the two fluid nozzle to work with viscous sample materials.
Nozzle set 1.4 mm titanium, complete
046380
11056415
Nozzle exchange set 2.0 mm, complete
Wider diameter for the two fluid nozzle to work with viscous sample materials.
046381
76/90 Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG
Nozzle set 2.0 mm titanium, complete
Nozzle cleaning acid proof
Nozzle needle
Needle 0.5 mm
Needle 0.7 mm titanium
Needle 1.4 mm
Needle 1.4 mm titanium
Needle 2.0 mm
Needle 2.0 mm titanium
Needle 0.7 mm
Needle 0.7mm titanium
Needle for nozzle cleaning
11056417
046373
11056422
046554
11056969
044618
Order no.
11056416
11059876
Order no.
11056864
11056315
046372
Appendix | 12
Image
Image
Operation Manual MiniSprayDryer S-300 77/90
12 | Appendix
Nozzle tip
Nozzle tip 0.5 mm
Nozzle tip 0.7 mm
Nozzle tip 0.7 mm titanium
Nozzle tip 1.4 mm
Nozzle tip 1.4 mm titanium
Nozzle tip 2.0 mm
Nozzle tip 2.0 mm titanium
Nozzle cap
Nozzle cap 1.4 mm
Nozzle cap 1.5 mm
Nozzle cap 1.5 mm titanium
Order no.
11056865
Büchi Labortechnik AG
Image
044634
11056317
046376
11056419
046377
11056424
Order no.
044649
044647
11057509
Image
78/90 Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG
Nozzle cap 2.2 mm
Nozzle cap 2.2 mm titanium
Nozzle cap 2.8 mm
Nozzle cap 2.8 mm titanium
Order no.
046374
11057510
046375
11057511
Appendix | 12
Image
O-rings nozzle
Set of O-rings for nozzle
Order no.
044759
O-ring for nozzle, FKM (green), 2× 044645
O-ring nozzle cap silicone (red), 2× 16.0 × 2.0 mm 002103
O-ring for needle and nozzle tip, FKM (green), 4×
6.0×1.5 mm
004222
O-ring for nozzle cleaner, FKM (black), 2× 3.0×1.5
mm
038348
O-ring FFKM for screw coupling 046363
O-ring for nozzle tip, FFKM (green), 2× 046361
Image
Operation Manual MiniSprayDryer S-300 79/90
12 | Appendix
12.2.2 Accessories
Inert Loop B-295 Upgrade box
Dehumidifier S-396 200 V
Dehumidifier S-396 220 V
Dehumidifier S-396 210 V
Dehumidifier S-396 230 V
Dehumidifier S-396 240 V
Inert Loop S-395 200V 50Hz
Inert Loop S-395 230V 50 HZ
Inert Loop S-395 200V 60 HZ
Inert Loop S-395 230V 60 HZ
Cable product cover
Ground pin Ø4 casing coated
80/90
11074622
11074623
11071611
11071709
Order no.
11074892
11073817
Büchi Labortechnik AG
Image
11074006
11073816
11073814
11073815
11074620
11074621
Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG
Inert gas adapter S-300, complete
Trolley S-300
Protective curtain right, complete
Protective curtain left, complete
Ultrasonic package
Peristaltic pump external
Second peristaltic pump for three fluid nozzle, nozzle cooling or shorter distance between pump and nozzle.
11070786
011235 Inlet filter, complete
Protects the sample from particles of the environmental drying air. Only for open mode.
Spray cylinder chrome steel kp 11064367
Adapter USB-Wi-Fi/Bluetooth 11072500
Oil-free compressor, 230 V/50 Hz
Compressed air maintenance unit
Oil-free compressor, 230 V/60 Hz
027907
004366
11055737
Order no.
11074499
11074575
11071754
11071651
11069892
Appendix | 12
Image
Operation Manual MiniSprayDryer S-300 81/90
12 | Appendix
12.2.3 Glassware
Glass assembly
Glass assembly S-300, complete
Order no.
11071071
11073658 Glass assembly S-300 brown, complete
Glass assembly corrosive S-300, complete 11071420
Büchi Labortechnik AG
Image
82/90
Glass assembly S-300 HP cyclone, complete 11074494
Glass assembly S-300 HP cyclone brown, complete
11074495
Cyclone
Standard cyclone
Order no.
004189
Image
Cyclone brown
High-performance cyclone
High-performance cyclone, brownglass
Cyclone with SVL 42
High performance cyclone, complete
11073659
046368
11056879
11071060
11074500
Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG
Order no.
High performance cyclone brown glass, complete 11074496
Spray cylinder
Spray cylinder
Order no.
044673
Spray cylinder brown glass
Spray cylinder, vertical outlet
044726
044697
Spray cylinder, vertical outlet. brown glass 044728
Cylinder insulation 040058
Appendix | 12
Image
Image
Collection vessel
Order no.
Large collection vessel for standard cyclone 1.1 L 11056990
Large product collection vessel for HP cyclone, complete
11056899
Cover for large collection vessel HP cyclone 11056901
Product collection vessel, brown glass
Product collection vessel
044727
044678
Image
Operation Manual MiniSprayDryer S-300 83/90
12 | Appendix
Small product collection vessel for HP cyclone
Order no.
046367
Büchi Labortechnik AG
Image
Other glassware related spare parts
Angle tube
Angle tube brown
Angle tube for HP cyclone
Angle tube for HP cyclone brown
Cap nut for cyclone
Cover product vessel for cyclone
Cover product vessel
Coupling flange
Coupling flange corrosives
Knurled handle with recess
Order no.
11070485
11073660
11073621
11074322
11070711
11072625
11071425
11073537
11071421
11071059
Image
84/90 Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG
Gasket SVL 42x35
O-Ring 104 x 6.99 FKM 70
Screw cap SVL 42
Separation flask
Push in connect NPQH-D-G1/8 Ø6
Separation flask
Gasket FPM to waste vessel
Silicone seal SVL 42
Holder to spray cylinder
O-ring to spray cylinder
Screw to holder
Cover to product collection vessel
Operation Manual MiniSprayDryer S-300
044711
044712
046318
004343
040471
040674
044710
Order no.
11071061
11071062
003551
004188
11071105
Appendix | 12
Image
85/90
12 | Appendix
Plastic closure for product collection vessel
Order no.
046358
Büchi Labortechnik AG
Image
12.2.4 Spare parts
Set O-ring Plastiperfl. S-300
O-ring Ø 5.00x1.50 Plastip.
Ventilation hose aspirator, complete
Hose clamp
O-Ring Ø 27.94x5.33 FKM 75
Quick release clamp
Clamping lever M4
Cover cap Ø 25.4
Gasket SVL 42x35 PTFE
Fixing nut T-sensor
11071080
11071171
11071194
11071325
11073019
Order no.
11074501
11071708
11074587
11071064
11071067
11071073
Image
86/90 Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG
Heater 2.3 kW 200 VAC conf.
Outlet filter, complete
Outlet filter corrosive, complete
PTFE membrane filter with clamp
Polyester filter bags (6 units)
Filter holder grounded
Adapter T-Sensor Outlet
Pt1000 Temp. sensor 380mm coat
Pt1000 Temp. sensor 380mm
Silicone tube for nozzle cooling, 4 m
11073020
11071407
11072982
004139
Order no.
11071353
11071410
11071411
11075115
035004
11073770
Appendix | 12
Image
Tygon tube MH2375 transparent (per m) 046314
Tygon tube F 4040 A yellow (per m) 046315
12.2.5 Hoses
Set tube PTFE
Order no.
11072713
Image
Operation Manual MiniSprayDryer S-300 87/90
12 | Appendix
Set tube PTFE corr.
Tube Inert Loop PTFE conf.
Hose Inert Loop TPR conf.
Set hose TPR corr.
Hose filter conf.
Set hose dry gas TPR
Set tubes for chiller
Hose filter conf. corr.
Hose TPR 0.7 m conf.
Hose TPR 0.7 m conf.
Hose TPR 1.0 m conf.
Hose PTFE 0.7 m conf.
Order no.
11072714
Büchi Labortechnik AG
Image
11071602
11071076
11071432
11071057
11071431
11073021
11071413
11071051
11071052
11071053
11071054
88/90 Operation Manual MiniSprayDryer S-300
Büchi Labortechnik AG
Hose PTFE 0.7 m conf.
Hose PTFE 1.0 m conf.
Hose TPR 0.7 m conf. coated
Hose TPR 0.7 m conf. coated
Hose TPR 1.0 m conf. coated
Hose PTFE 0.7 m conf. coated
Hose PTFE 0.7 m conf. coated
Hose PTFE 1.0 m conf. coated
12.2.6 Documents
Set IQ/OQ S-300 en
Repeating OQ S-300 en
Order no.
11071055
11071056
11071603
11071604
11071605
11071606
11071607
11071608
Appendix | 12
Image
Order no.
11074567
11074568
Operation Manual MiniSprayDryer S-300 89/90
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