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5  Putting into operation

55

B-90

 Operation Manual, Version B

5.7.2 

Aspirator in ‘closed loop’ configuration

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

a

b

c

d

a

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

or Dehumidifier B-296)

b

  Gas outlet towards gas inlet connector of the Nano 

Spray Dryer B-90 in Polypress design

c

  Output flow-through selector (frequency based 

regulation)

d

  Mains socket, switch and fuse box

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

Installation steps
1.  Disconnect the power cord from the mains and depressurize all system parts.
2.  Connect the gas inlet a to the outlet of Inert Loop B-295 or Dehumidifier B-296.
3.  Connect the gas outlet b to the GAS IN connection of Nano Spray Dryer B-90 Advanced.
4.  Connect the power cord to the mains. The device can now be switched on.

NOTE 

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

5.8 

Inert Loop B-295 installation

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

!

 

Danger

Death by suffocation or serious poisoning by inhalation of inert gases.
•  Do not inhale inert gases
•  Directly withdraw released gases and gaseous substances by sufficient ventilation
•  Only operate the instrument in ventilated environments
•  Before operation, check all parts, connections and sealings involved in the gasflow for proper 

sealing

•  Exchange worn out or defective parts immediately

Summary of Contents for Nano B-90

Page 1: ...093261 en Nano Operation Manual Spray Dryer B 90...

Page 2: ......

Page 3: ...his manual 6 2 Safety 7 2 1 User qualification 7 2 2 Proper use 7 2 3 Improper use 8 2 4 Safety warnings and safety signals used in this manual 8 2 5 Product safety 10 2 5 1 General hazards 10 2 5 2 W...

Page 4: ...Outlet filter installation replacement 53 5 7 Aspirator installation modes 54 5 7 1 Aspirator in open loop configuration 54 5 7 2 Aspirator in closed loop configuration 55 5 8 Inert Loop B 295 instal...

Page 5: ...85 7 6 2 Outlet filter 86 7 6 3 Inert Loop B 295 and Dehumidifier B 296 86 8 Troubleshooting 87 8 1 Error messages and their remedy 87 8 2 Malfunctions and their remedy 89 9 Shutdown storage transpor...

Page 6: ...all information required for its safe operation and to maintain it in good working order It is addressed to laboratory personnel in particular Abbreviations EPDM Ethylene Propylene Dimonomer FFKM Perf...

Page 7: ...tions or suspensions in open loop with compressed air as drying gas The Nano Spray Dryer B 90 Advanced can additionally process organic solvent solutions or suspensions in closed loop when combined wi...

Page 8: ...e standardized signal words for identifying levels of hazard seriousness of risks related to personal injury and property damage All signal words which are related to personal injury are accompanied b...

Page 9: ...list incorporates all safety information symbols used in this manual and their meaning Symbol Meaning General warning Electrical hazard Explosive gases explosive environment Harmful to life forms Hot...

Page 10: ...gs in this manual as described in section 2 4 serve to make the user alert and to avoid hazardous situations emanating from residual dangers by giving appropriate counter measures However risks to use...

Page 11: ...serious poisoning by gases or particles due to O2 sensor or filter malfunction Exchange defective O2 sensor immediately Exchange O2 sensor regularly within the specified maintenance intervals Exchang...

Page 12: ...instrument in explosive environments Do not operate the instrument with explosive gas mixtures Before operation check all gas connections for correct installation Directly withdraw released gases and...

Page 13: ...its component parts Wipe off any liquids instantly Place the sample vessel onto the designated reservoir plate on top of the instrument Ensure a safe positioning of the sample vessel Do not move the i...

Page 14: ...tective eye goggles protective clothing inha lation protection and gloves when working with the instrument 2 5 4 Built in safety elements and measures Heating Overheating protection circuit Automatic...

Page 15: ...l regulations such as local state and federal laws applying to the instrument must be strictly followed Duty of maintenance and care The operator is responsible for the proper condition of instrument...

Page 16: ...90 Advanced For solvent applications in combination with Inert Loop B 295 Optional use with Dehumidifier B 296 Equipped with additional oxygen safety circuit and gas regulation valves Accessories are...

Page 17: ...Standard accessories Product Order no Spray head 051510 Spray head holder 051508 3 Set of 3 spray caps 4 0 m 051747 Set of 3 spray caps 5 5 m 051748 Set of 3 spray caps 7 0 m 051749 HV Electrode prot...

Page 18: ...sion B 1 Table 3 2 Standard accessories cont Product Order no Spray cylinder 051511 Glass cylinder extension 051549 Glass insulation cylinder no picture 051663 Heater complete 051504 Lifting device 05...

Page 19: ...Advanced Table 3 3 Standard accessories with the B 90 Advanced for closed loop operation Product Order no Oxygen sensor 046348 Tygon tubing MH 2075 transparent per m 046314 Tygon tubing F 4040 A yell...

Page 20: ...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...

Page 21: ...peration Manual Version B Table 3 4 Optional accessories cont Product Order no Inlet filter 011235 Air maintenance unit 004366 Oil free air compressor 230V 50Hz 027907 Oil free air compressor 230V 60H...

Page 22: ...m Mean droplet size range 8 21 m Mean particle size range 300 nm 5 m Mean residence time 1 4 sec Interface USB II IP degree of protection two digits IP 42 Explanation of protection level 4 Protection...

Page 23: ...ehumidifier B 296 Power consumption 700 W Connection voltage 200 230 V 10 Frequency 50 60 Hz Min outlet temperature 2 C Rate of cooling 600 W at 0 C Dimensions W H D 35 40 60 cm Weight 36 kg Table 3 8...

Page 24: ...3 3 borosilicate glass Heater Aluminum and stainless steel Spray head Stainless steel Spray cap membrane Stainless steel Spray cap o ring EPDM75 Feeding tubes Silicone and tygon Tube connector at fee...

Page 25: ...transport gas enters the instrument via the Drying gas inlet b The gas flow is monitored by a Flow meter which influences the Gas regulator c Subsequently the Electrical heater heats up the gas to th...

Page 26: ...gas flow The following scheme informs about the different processing stages in general Drying gas inlet Flow meter Electrical heater Inlet temp sensor c Drying cylinder d Electrical particle collecto...

Page 27: ...lecting electrode i HV electrode j Outlet temperature sensor k Outlet filter l Drying gas outlet in closed loop connected to Inert Loop B 295 and Aspirator 4 2 Spray generation The Nano Spray Dryer B...

Page 28: ...l air maintenance unit c Pressure regulating valve 4 4 2 Aspirator in blowing mode If there is no compressed air available in the laboratory the BUCHI Aspirator unit with inlet filter order no 051700...

Page 29: ...ple feed circulation with peristaltic pump The peristaltic pump circulates the sample feed between the product vessel and the spray head It assures a constant substance feeding for the spray generatio...

Page 30: ...rying gas N2 or CO2 is loaded with solvent from the spray drying process The loaded gas enters the Inert Loop B 295 and is cooled down in its internal preheat exchanger The solvent is condensed in the...

Page 31: ...tioning In open loop configuration with Aspirator and Inlet filter the Dehumidifier B 296 has to be connected to the gas inlet of the Nano Spray Dryer B 90 for inlet air conditioning The dried cooled...

Page 32: ...flask d Aspirator to establish gasflow e Dongle to substitute the missing Inert Loop B 295 signals Suitable spray drying conditions Water organic solvent mixture with up to 20 organic solvent content...

Page 33: ...the dongle to substitute missing communication when operating with Dehumidifier B 296 d USB Port for data records to PC Rear and side connections Socket label Description e GAS OUT Gas outlet exhaust...

Page 34: ...ossible Obtain the environmental conditions as described in section 3 2 technical data NOTE T o cut the power in case of an emergency by unplugging the instruments or any other items must not block th...

Page 35: ...wrench to screw them tightly in d Screw the middle metal bars tightly onto the lower ones e Mount four short headless screws onto the middle metal bars Use a hex wrench to screw them tightly in f Scre...

Page 36: ...e lower metal bars Use a hex wrench to screw them tightly in d Screw the middle metal bars tightly onto the lower ones e Mount the four long headless screws onto the upper metal bars Use a hex wrench...

Page 37: ...and The lever has to be positioned towards the front d e c 70 mm c Screw the gas outlet part onto the lifting device with two hex wrench screws d Take the small o ring from the set of sealings order n...

Page 38: ...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 b Position the metal col...

Page 39: ...ector 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 HV electrode in a vertical upward...

Page 40: ...te cuts when handling damaged glass parts Handle glass parts with care Visually inspect every glass part before mounting Exchange damaged glass parts immediately Do not touch cracks or bits of broken...

Page 41: ...minor or moderate burning when handling hot parts Do not touch hot parts Let the system cool down for some minutes after use 2 5 The special mounting tool serves as a mounting gauge for the correct d...

Page 42: ...ure the spray cylinder is in line with the heater module and that the sealing is properly placed between e f Tighten the hex counter nuts above and below the heater crosswise Do not overtighten the nu...

Page 43: ...arts during assembling and installation are required For detailed cleaning information see section 8 6 1 Caution Risk of minor or moderate burning when handling hot parts Do not touch hot parts Let th...

Page 44: ...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 sea...

Page 45: ...l cable e and tighten the cable bushing using a flat spanner 6 Introduce the Feed tubing j through the spray head 7 Screw the Spray cap k onto the spray head 8 Introduce the Feed tubing k into the Fit...

Page 46: ...BUCHI torque wrench to fasten the spray cap at the spray head with a torque of 7 Nm 15 Remove the spray head with the mounted spray cap from the mounting tool 16 Remove the mounting tool from the meta...

Page 47: ...gle 30 45 or 60 and reattach the screw in the chosen angle Fasten the screw again To mount the spray head use a small torx screw M3 16 to fix it at the holder b For vertical spray head position To mou...

Page 48: ...mps 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 Pre adjust the pump bed...

Page 49: ...e tygon type for other solvents see also Table 5 1 for a list of most common solvents Sample vessel 1 2 a Install the feeding tube at the peristaltic pump first Make sure the plastic manifold is seate...

Page 50: ...075 Tygon F 4040 A Methanol suitable suitable suitable Ethanol suitable suitable suitable Acetone unsuitable suitable unsuitable Toluene unsuitable unsuitable suitable Isopropanol suitable suitable su...

Page 51: ...he gasflow for proper sealing Exchange worn out or defective parts immediately Warning Death or serious poisoning by contact or incorporation of harmful substances at use Before operation check the in...

Page 52: ...nd supply tubes NOTE If there is no compressed air available the compressed air can also be supplied by an oil free compressor a b c a Coarse filter b Submicron filter c Activated charcoal filter The...

Page 53: ...as flow a GAS OUT Polypress with clamp fitting b N2 quick coupling c AIR CO2 quick coupling d GAS IN Polypress with clamp fitting 5 6 3 Outlet filter installation replacement The Nano Spray Dryer B 90...

Page 54: ...the required instrument input pressure for the drying medium flow the output of the Aspirator can be used in blowing mode The Aspirator can be part of an open loop configuration In closed loop the us...

Page 55: ...e gas outlet b to the GAS IN connection of Nano Spray Dryer B 90 Advanced 4 Connect the power cord to the mains The device can now be switched on NOTE The Aspirator can not be used in combination with...

Page 56: ...sed gas Depressurize gas circuit before any modification work Wear safety goggles Warning Death or serious poisoning by contact or incorporation of condensed liquid Dispose of condensate safely after...

Page 57: ...essure check valve hose connectors and compressed gas tubing for CO2 and N2 c b a a Communication cable to the Nano Spray Dryer B 90 Advanced see section 4 10 socket c b Oxygen concentration display w...

Page 58: ...switched on NOTE If air is sucked in through the tube during operation this is an indication that the closed loop is not tight Switch off the assembly and re check all connections and sealings immedia...

Page 59: ...the mains and depressurize all system parts 2 Place the Dehumidifier B 296 next to the Nano Spray Dryer B 90 and the Aspirator 3 Connect the tubing from the outlet labelled on the enclosure of the De...

Page 60: ...of the Dehumidifier B 296 to the gas inlet of the Aspirator see section 5 6 1 connector a An additional tube is needed 4 Connect the Aspirator outlet to the inlet of the Nano Spray Dryer B 90 see sect...

Page 61: ...he tubing 6 Connect the outlet of the Inert Loop B 295 to the inlet of the Aspirator see section 5 6 1 gas inlet a Use hose clamps to fix the tubing 7 Connect the gas outlet of the Aspirator to the GA...

Page 62: ...30 to 60 mbar for a well sealed system in open loop 5 11 Electrical connections After the installation procedure and the final check has been completed successfully the power plug of the Nano Spray Dr...

Page 63: ...n at their main switch 6 2 Main screen After the internal system check at bootup finished successfully the main screen view below appears at the Nano Spray Dryer B 90 a b c d e f g h i a Display showi...

Page 64: ...as inlet temperature between 0 C to 120 C NOTE The lowest possible drying gas inlet temperature in open loop mode depends on the local room temperature 6 3 Menu structure overview The table below show...

Page 65: ...able 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...

Page 66: ...uttons 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 o...

Page 67: ...elect Gas mode and enter the selection Select the correct setting for the actual spray drying process and confirm the selection with OK NOTE Set to Air for open loop mode Set to 4 O2 for closed loop m...

Page 68: ...ssure in mbar Torr hPa LCD Contrast Select a screen contrast between 0 and 100 Sea level Select the sea level in meters over sea level Rot release Defines the time interval in which the rotary knob is...

Page 69: ...e 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 dryin...

Page 70: ...e automatic self check the operating mode is activated 2 Switch on all other devices if installed in the current configuration 3 Set the drying gas rate to a reasonable flow of about 70 150 liter min...

Page 71: ...um inlet drying gas temperature To reduce the thermal load on the feed the sample vessel maybe cooled The achievable droplet sizes depend on the installed spray cap Mean values for water applications...

Page 72: ...F the peristaltic pump afterwards and lower the pump bed to release the mechanical load of the pulleys at the tube 6 See section 6 8 before open the glass assembly in safe environment prior to any par...

Page 73: ...eet of paper into a storage vessel Depending on the substance a particle recovery rate of up to 90 can be achieved NOTE Act carefully e g avoid shaking movements in order to prevent loss of particles...

Page 74: ...e 4 O2 or 1 O2 in submenu 1 The instrument automatically detects the connected periphery 4 Switch on the Aspirator 5 Turn on the inert gases N2 and CO2 Set the CO2 pressure to maximal 2 bar and the ab...

Page 75: ...he kind of set up see section 5 for more information Carry out a final installation check see section 5 9 before every spray drying process Operate the Nano Spray Dryer B 90 Advanced in closed loop as...

Page 76: ...possi bility of cross contamination significantly 6 10 Using the Nano Spray Dryer Records software on a PC The PC software enables online data monitoring and storage of experimental runs in a virtual...

Page 77: ...ual Version B Initial view and program functions Menu bar entries Accessible sub entries File New LabBook Open LabBook Close LabBook Exit View Show tree Tools Selftest Options Help Contents Import Lic...

Page 78: ...to CSV Character Separated Values k Close Experiment l Delete Experiment LabBook entries Each experiment is stored as an entry in a LabBook In order to record an experiment a LabBook must already be...

Page 79: ...cording 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...

Page 80: ...old comments unique attributes for identification and information about the drying conditions and system settings This information will show up in PDF reports Select a LabBook and one or more experime...

Page 81: ...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...

Page 82: ...d on the screen of the Nano Spray Dryer B 90 At the end of the self test a PDF report is generated It can be used as a support tool by BUCHI representatives for service and trouble shooting NOTE The s...

Page 83: ...t need prior written permission of the manufacturer Danger Death or serious poisoning by inhalation or incorporation of dried particles during maintenance Wear safety goggles Wear safety gloves Wear a...

Page 84: ...customer service offices are given on the BUCHI website under www buchi com If malfunctions occur on your instrument or you have technical questions or applica tion problems contact one of these offic...

Page 85: ...ng the lifetime of the seals rinse them routinely with water or ethanol and always when there has been the possibility of unwanted sample contamination Dry the cleaned seals with a soft lint free clot...

Page 86: ...oop B 295 can be flooded completely for cleaning purpose Notice Risk of instrument and instrument damage by liquids and detergents Do not spill liquids over the instrument or parts of it Wipe off any...

Page 87: ...ray head plug is plugged in correctly Switch off the device and try again If the error still occurs replace the spray head or contact the BUCHI customer service 003 Resonance not found check the spray...

Page 88: ...ontact BUCHI customer service 023 Difference pressure sensor not connected Sensor not connected or defec tive internal wiring Contact BUCHI customer service BUCHI 024 Inside pressure low System not le...

Page 89: ...tion in process Connection cable plugged in after switching on the instrument Restart the system 203 Pressure alarm not given during start up Pressure switch defective or contaminated Contact BUCHI cu...

Page 90: ...lar or pulsed spraying Leaks in the spray head Check seal in the spray head and replace if necessary Deposits in the particle collector Product too moist Increase inlet temperature to dry the product...

Page 91: ...nd dusty residues before packaging the instrument Warning Death or serious poisoning by contact or incorporation of harmful substances Wear safety goggles Wear safety gloves Wear a suitable protective...

Page 92: ...r 3 This helps to ensure that the components can be separated and recycled correctly You have to follow valid regional and local laws concerning disposal For help please contact your local authorities...

Page 93: ...ed in the laboratory and is new was not in contact with toxic corrosive biologically active explosive radioactive or other dangerous matters is free of contamination The solvents or residues of pumped...

Page 94: ...designation instrument serial and part numbers for warranty clearance when ordering spare parts 10 1 Spray head Table 10 1 Spray head Description Order no Spray head 051510 Spray head holder 051508 S...

Page 95: ...n B 10 2 Glass parts and mounting items Table 10 2 Glass parts and mounting parts Description Order no Spray cylinder 051511 Glass cylinder 051549 Sealing set complete 051778 Tool box B 90 051767 Cent...

Page 96: ...ticle collecting tube 051662 Glass insulation tube 051663 Collector base complete 051669 Nano particle scraper 11055338 Particle collection paper 100 pages 11055339 Heater complete 051504 Set of 3 pol...

Page 97: ...scription Order no Gas inlet connection 051781 Polypress tube gas outlet 2 m 046329 Hose clamp 25 40mm 004236 Pressure relieve valve 11055829 Polypress tube quick coupling 045656 Compressed gas tube c...

Page 98: ...Nano Spray Dryer records 051776 USB Kabel 2 0 A B 2 0 m 11055310 USB Kabel 2 0 A B 4 5 m 049226 10 6 Inert Loop B 295 Dehumidifier B 296 and Adsorption Column 46348 04105 27338 40398 Table 10 7 Inert...

Page 99: ...oulff bottle 041875 b Screw cap SVL 22 003577 c Closed screw cap SVL 22 005222 Gasket 22 17 PTFE 005155 PFTE hose connection SVL 22 027338 Polypress tube 2m 046329 Hose clamp 25 40 mm 004236 Viton sea...

Page 100: ...ause harmful interference in which case the user will be required to correct the interference at his own expense Fran ais Cet appareil a t test et s est av r conforme aux limites pr vues pour les appa...

Page 101: ...11 Declarations and requirements 101 B 90 Operation Manual Version B 11 2 Declaration of conformity...

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Page 104: ...B CHI Labortechnik AG CH 9230 Flawil 1 Switzerland T 41 71 394 63 63 F 41 71 394 65 65 www buchi com Quality in your hands...

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