Operation Manual Nano Spray Dryer B�90 093261 en
Table of contents Table of contents 1 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 2 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 2.1 User qualification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 2.2 Proper use . . . . . . . . . . . .
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 . . . . . . . . . . . . . . . . . . . .
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 . . . . . . . . . . . . . . . .
1 About this manual 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.
2 Safety 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.
2 Safety 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.
2 Safety Table of supplementary safety information symbols The below reference list incorporates all safety information symbols used in this manual and their meaning.
2 Safety Wear laboratory coat Wear protective goggles Wear protective gloves Heavy weight, lifting requires more than one person 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.
2 Safety ! Danger Death by suffocation or serious poisoning by inhalation of inert gases.
2 Safety ! Danger Death or serious poisoning by inhalation or incorporation of dried particles at recovery.
2 Safety ! Caution Risk of minor poisoning by inhalation of ozone. • ! Directly withdraw released gases and gaseous substances by sufficient ventilation Caution Risk of minor or moderate burnings when handling hot parts. • • Do not touch hot parts Let the system cool down for some minutes after use Notice Risk of instrument short-circuits and damage by liquids.
2 Safety 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. 2.5.
2 Safety 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.
3 Technical data 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.
3 Technical data 3.1.2 Standard accessories Table 3-2: Standard accessories 3✕ 17 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.
3 Technical data Table 3-2: Standard accessories (cont.) Product Order no.
3 Technical data Table 3-2: Standard accessories (cont.) Product Order no. Outlet filter 051656 Operation Manual Nano Spray Dryer B�90 093261 Deckblatt B-90_en.indd 1 3.1.3 Operation Manual: English 093261 German 093262 French 093263 Italian 093264 Spanish 093265 en 08.07.2009 09:44:56 Standard accessories with the Nano Spray Dryer B-90 Advanced Table 3-3: Standard accessories with the B-90 Advanced (for ‘closed loop’ operation) Product Order no.
3 Technical data 3.1.4 Optional accessories Table 3-4: Optional accessories 20 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.
3 Technical data Table 3-4: Optional accessories (cont.) 21 Product Order no.
3 Technical data Table 3-4: Optional accessories (cont.) 3.2 Product Order no. Stand plate 051775 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 (higher rates with organic solvents are possible) Drying gas flow 80–160 l/min N2 or CO2 inert gas input pressure max.
3 Technical data 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 Short set-up 65 kg Tall set-up 70 kg Weight 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.
3 Technical data 3.3 Materials used Table 3-9: Materials used Component Material designation Glass assembly 3.
4 Description of function 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.
4 Description of function 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.
4 Description of function 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).
4 Description of function 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.
4 Description of function Nano Spray Dryer B-90 Basic T IN Dehumidifier B-296 Feed Control T COOL P c (optional) Aspirator b FI Product Condensate T OUT Exhaust gas Outlet filter a Inlet filter a Inlet filter to filter out dust and particles b Aspirator as air supply source c Optional Dehumidifier B-296 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 Description of function 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.
4 Description of function 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.
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.
4 Description of function 4.
5 Putting into operation 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.
5 Putting into operation 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. 9 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.
5 Putting into operation 5.2.2 Short set-up with short metal bars NOTE Parts (a – e) and the black holders (g), are factory pre-installed. 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.
5 Putting into operation 5.3 Sub-assembly installations Switch off the instrument and remove the power cord before any installation work. 5.3.1 Lifting device 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.
5 Putting into operation 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. a Position the flat seal at the particle collector basement.
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.
5 Putting into operation 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. 7 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. 5.3.
5 Putting into operation Cylinder assembly short set-up 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. 2 5 All sealings are part of the sealing set (order no. 051778). 5.3.4 Heater module installation ! Caution Risk of minor or moderate burning when handling hot parts.
5 Putting into operation 4 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.
5 Putting into operation 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. • • 5.4.
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.
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. Screw the “Spray cap” k onto the spray head. 7. 8. 9. 45 Introduce the “Feed tubing” k into the “Fittings” f. Attach the “Ferrules” h to the “Feed tubing”. Mout the “Tube connectors” i at the “Fittings”.
5 Putting into operation b a 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.
5 Putting into operation 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.
5 Putting into operation 5.5.1 Peristaltic pump height adjustment and fixation 3 1 2 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 1 2 a Turn the lever horizontally to the left.
5 Putting into operation 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). 1 2 Sample vessel a Install the feeding tube at the peristaltic pump first.
5 Putting into operation Example photo with attached feeding tube and adapter piece (transparent adapter on the pump inlet at the right side).
5 Putting into operation 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. ! Danger Death by suffocation or serious poisoning by inhalation of inert gases.
5 Putting into operation 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).
5 Putting into operation 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. The drying gas connections are located on the right side of the instrument (see section 4.
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.
5 Putting into operation 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 ! 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.
5 Putting into operation 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.
5 Putting into operation Installation steps 1. 2. 3. 4. 5. Disconnect the power cord from the mains and depressurize all system parts. Install the check valve at the exhaust gas tubing outlet and lead it to a fume hood or ventilation system. Connect all tubes (see pictures). Connect the communication cable to the Nano Spray Dryer B-90 Advanced. Connect the power cord to the mains. The device can now be switched on.
5 Putting into operation 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. a Input/Output gas connectors (Polypress style) a b System status display c Power switch d Attached condensate vessel b c d Installation steps 1. 2. 3. 4. 5. 6.
5 Putting into operation 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.
5 Putting into operation 1 2 3 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. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 61 Disconnect the power cord from the mains and depressurize all system parts. Put the holder of the adsorption column e on the Inert Loop B-295 and fix it with the adhesive tape. Attach the adsorption column with the installed sieve bag and the humidity sensor a at the holder e.
5 Putting into operation 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.
6 Operation 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 • • • • 6.2 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.
6 Operation 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.
6 Operation 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 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.
6 Operation 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 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 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. Items in menu “Configuration”: Description / available parameters: Units • • • LCD-Contrast Select a screen contrast between 0 and 100 %. Sea level Select the sea level in meters over sea level. Rot.
6 Operation 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. z NOTE The calibration should be performed periodically to ensure best spray drying results. 6.4.
6 Operation 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.
6 Operation 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.
6 Operation 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. 2. 3. 4. 5. 6. 6.8 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. Switch off the spray head by pressing the “Spray” button.
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. 2. 3. 4. 5. 6.
6 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.
6 Operation 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.
6 Operation 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.
6 Operation Initial view and program functions Menu bar entries: 77 Accessible sub entries: File • • • • New LabBook Open LabBook Close LabBook Exit View • Show tree Tools • • Selftest Options Help • • • • Contents Import License Software registration About B-90 Operation Manual, Version B
6 Operation Tool bar functionality a b c d e f g h i j k l Tool bar items: Tool functionality: a Start/Stop recording b New LabBook c Delete LabBook d Open existing LabBook e Close LabBook f Import LabBook g Export LabBook h Open Experiment i Show Report (Create a pdf-file with a choosen data set) j Export to CSV (Character-Separated Values) k Close Experiment l Delete Experiment LabBook entries Each experiment is stored as an entry in a LabBook.
6 Operation Program options The program can be configured in the “Options” menu. • • • • • 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.
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. • • 80 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.
6 Operation Access recorded data Recorded spray drying data can be displayed in plot or table view. 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”.
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.
7 Maintenance and repairs 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.
7 Maintenance and repairs ! Warning Death or serious injuries by compressed air and gases. • • Depressurize air and gas circuit first Wear safety goggles Notice Risk of instrument and instrument damage by liquids and detergents. • • • 7.1 Do not spill liquids over the instrument or parts of it Wipe off any liquids instantly Use ethanol or soapy water as detergent only Customer service Only authorized service personnel are allowed to perform repair work on the instrument.
7 Maintenance and repairs ! Caution Risk of minor or moderate cuts when handling damaged glass parts. • • • • 7.4 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 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.
7 Maintenance and repairs 7.6.2 Outlet filter A clogged outlet filter results in a pressure drop between inside the Nano Spray Dryer B-90. Notice Risk of instrument damage by internal overpressure. • • • • • 7.6.
8 Troubleshooting 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.
8 Troubleshooting Table 8-1: Error messages and their remedy (cont.) 011 Inlet temperature exceeded Heating control or heating relais defective Switch off the device and try again. If the error still occurs replace the heater module or contact the BUCHI customer service. 014 Voltage HV-Module HV-module defect or internal wiring interruption or quality falloff voltage because of a short circuit Switch off the device and try again. If the error still occurs contact the BUCHI customer service.
8 Troubleshooting Table 8-1: Error messages and their remedy (cont.) 043 O2 sensor short-circuit Defective sensor, sensor cable or Contact BUCHI customer service internal wiring 046 O2 concentration high System not leakproof, N2-bottle empty Test for leakages. Check system sealings and N2-supply. 047 O2 concentration low Valve defective Contact BUCHI customer service 050 B-295 O2 concentration too high System not leakproof, N2-bottle empty Test for leakages.
8 Troubleshooting Table 8-2: Malfunctions and their remedy (cont.
9 Shutdown, storage, transport and disposal 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.
9 Shutdown, storage, transport and disposal 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.
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.
10 Spare parts 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.
10 Spare parts 10.2 Glass parts and mounting items Table 10-2: Glass parts and mounting parts 95 Description Order no.
10 Spare parts 10.3 Particle collector, heater and lifting device items Table 10-3: Electrical particle collector, heater and lifting device Description Order no.
10 Spare parts 10.4 Filters Table 10-4: Outlet filter Description Order no. Outlet filter 051656 Table 10-5: Inlet filter 10.5 Description Order no. Inlet filter complete 011235 Replacement filter with seal 011238 Tube Flexflyte D51mm (0.8 m) 011240 Tubing and accessories Table 10-6: Tubing 97 Description Order no.
10 Spare parts Table 10-6: Tubing (cont.) 10.6 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.
10 Spare parts Table 10-7: Inert Loop B-295, Dehumidifier B-296 and Adsorption column (cont.) 99 Description Order no.
11 Declarations and requirements 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.
11 Declarations and requirements 11.
BÜCHI Labortechnik AG CH-9230 Flawil 1 / Switzerland T +41 71 394 63 63 F +41 71 394 65 65 www.buchi.