Synthos 3000 Reference Manual

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Reference Manual Synth yn thos os 3000 Microwave Synthesis

Anton Paar GmbH assumes no liability for technical or printing errors or omissions in this document. Nor is any liability assumed for damages resulting from information contained in the document. Anton Paar GmbH reserves the right to content changes. This also extends to changes to delivery volumes or any features of delivered parts. All rights reserved (including translation). This document, or any part of it, may not be reproduced, changed, copied, or distributed by means of electronic systems in any form (print, photocopy, microfilm or any other process) without prior written permission by Anton Paar GmbH. Trademarks, registered trademarks, trade names, etc. may be used in this manual without being marked as such. They are the property p roperty of their respective o wner. Published by Anton Paar Printed: Anton Paar, Austria Copyright © 2006 Anton Paar GmbH, Graz, Austria Address:

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Date: 12.2006 Document number C49IB08A

1 Intr od uc ti on .............. .................... ............ ............. ............. ............ ............. ............. ............. ............. ............ ............. ............. ............ ............. ............. ............. ............. ............ ........... ..... 5 2 Symb ol s ............. ................... ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. .............. .............. ............. ............. ............. ............ ............ ......... ... 6

2.1 Symbols Symbols in in the Instruction Instruction Manual Manual ................ ....................... ............. ............. .............. .............. ............. ............. .............. ............. ............. .............. ....... 6 2.2 Safety Symbols Symbols Applied Applied to the the Instrumen Instrumentt ............... ...................... .............. ............. ............. .............. ............. ............. .............. ............. ......... ... 6 3 Safety Ins tr uc ti on s ........... .................. .............. ............. ............. ............. ............. ............. ............. .............. ............. ............. ............. ............. .............. ............ ............ ............. ...... 8 3.1 General Safety Instructions Instructions for Synthos Synthos 3000 .................. ......................... ............. ............. ............. ............. ............. ............. ............. ........ .. 9 3.2 Safety Instructions Instructions for Chemical Chemical Synthesis Synthesis ............. ................... ............. ............. ............. ............. ............. ............. ............. ............. ......... ... 12 3.3 Unexpected Unexpected Operation Operation Behavior Behavior ....... .............. .............. ............. ............. .............. ............. ............. .............. ............. ............. .............. .............. .......... ... 14 4 Techn ic al Descr ip ti on of Syn th os 3000 .......... ................ ............. .............. ............. ............. .............. ............. .............. ............... .............. .............. ......... 17 4.1 4.2 4.3

Working Working Princip Principle le ................ ...................... ............. .............. ............. ............. ............. ............. ............. ............. .............. ............. ............. ............. ............ ............. ....... 17 Fields Fields of Applicati Application on ............ .................. ............. ............. ............. .............. ............. ............. ............. ............. .............. ............. ............. .............. ............. ............ ...... 18 Technical echnical Descript Description ion of the Instrum Instrument ent .............. ..................... ............. ............. .............. .............. ............. ............. ............. ............. ............. ...... 19 4.3.1 Microwave Microwave Heating Heating ............. .................... ............. ............. .............. ............. ............. ............. ............. ............. ............. .............. .............. .......... ... 22 4.3.2 Magnetron Magnetron Protection Protection ............. ................... ............. ............. ............. .............. ............. ............. ............. ............. ............. ............. .............. ....... 22 4.3.3 4.3.3 Unpuls Unpulsed ed Energy Energy Contro Controll ....... .......... ...... ....... ....... ...... ...... ....... ....... ...... ....... ........ ....... ....... ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ...... .. 22 4.3.4 Safety Features Features ............. .................... .............. .............. .............. ............. ............. ............. ............. .............. ............. ............. ............. ............. ......... 23 4.3.5 4.3.5 Coolin Cooling g and Exhaus Exhaustt ....... ........... ....... ...... ....... ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ....... ....... ........ ....... ...... ....... ....... ...... ....... ........ ....... ..... 26 4.3.6 Rotor Detection Detection .............. ..................... ............. ............. ............. ............. ............. ............. .............. ............. ............. ............. ............. .............. ......... 27 4.4 Technical echnical Descrip Description tion of of the IR Tempe Temperature rature Sensor Sensor Accessor Accessory y ............. .................... ............. ............. .............. ......... .. 30 4.5 Technical echnical Description Description of the Pressure Pressure /Temper /Temperature ature Sensor Accessory Accessory .............. ..................... .............. ......... .. 31 4.5.1 4.5.1 Pressu Pressure re Measur Measureme ement nt ....... ........... ........ ........ ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ..... 33 4.5.2 Temperature emperature Measureme Measurement nt ............. .................... ............. ............. .............. ............. ............. .............. ............. ............. .............. .......... ... 34 4.6 Technical echnical Descript Description ion of the T-Probe T-Probe ............... ..................... ............. ............. ............ ............. ............. ............. ............. ............ ............. ............ ..... 36 4.6.1 Temperature emperature Measuremen Measurementt ............. .................... ............. ............. ............. ............. .............. ............. ............. .............. .............. .......... ... 37 4.7 Technical echnical Description Description of the the Safety Safety Module Module SOL SOLV V ............. .................... ............. ............. ............. ............. .............. .............. .......... ... 38 4.8 Technical echnical Descrip Description tion of the Solvent Solvent Sensor Sensor Access Accessory ory ............. .................... ............. ............. .............. ............. ............. ......... .. 39 4.8.1 Installation Installation ............. ................... ............. .............. .............. ............. ............. .............. ............. ............. ............. ............. ............. ............. .............. .......... ... 39 4.8.2 Function Function Verifica Verification tion ............ ................... ............. ............. ............. ............. .............. ............. ............. .............. ............. ............. ............. ......... ... 41 4.9 Technical echnical Descript Description ion of the Magneti Magnetic c Stirrer Stirrer Device Device ............. ................... ............. ............. ............. ............. ............. .............. ......... 45 5 Inst allat io n ............. ................... ............. ............. ............. ............. ............. .............. ............. ............. ............. ............. .............. .............. .............. ............. ........... ............ .............. ......... .. 46 5.1

Installati Installation on Requirement Requirements s .............. ..................... .............. .............. ............. ............. ............. ............. ............. ............. ............. ............. .............. ............. ........ 46 5.1.1 Exhaust Exhaust System .............. ..................... ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. .............. ............. ........ 46 5.1.2 5.1.2 Electr Electrica icall Requir Requireme ements nts ....... ........... ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ...... 47 5.2 Installati Installation on Steps Steps ................. ....................... ............. .............. ............. ............. .............. .............. ............. ............. ............. ............. .............. ............. ............ ............ ...... 48 5.3 Connecting Connecting Accessories Accessories ........... .................. .............. ............. ............. ............. ............. .............. .............. .............. .............. ............. ............. ............. ........... ..... 51 5.3.1 Printer Printer ............. ................... ............. ............. ............. ............. ............. ............. ............. ............. ............. .............. ............. ............. ............. ............. ............ ..... 51 5.3.2 Keyboard Keyboard ............. ................... ............. ............. ............. .............. ............. ............. ............. ............. .............. ............. ............. ............. ............. ............. ...... 51 5.3.3 External External Computer Computer ............. .................... .............. .............. ............. ............. ............. ............. .............. .............. ............. ............. ............. ......... ... 51 5.4 Activating Activating / Deactivating Deactivating Rotors, Rotors, Sensors Sensors and Accessorie Accessories s ............. .................... .............. .............. ............. ............. ......... .. 52 5.5 Microwave Microwave Power Calibration Calibration ................ ...................... ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ......... 53 6 Soft ware ............. .................... ............. ............. .............. ............. ............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ............ ............ ............ ............ ...... 58 6.1 6.2 6.3 6.4 6.5 6.6

General General Inform Information ation ............ ................... ............. ............. ............. ............. .............. .............. ............. ............. .............. ............. ............. ............. ............ ............ ...... 58 Basic Software Software Structur Structure e ............. .................... .............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. .............. .......... ... 60 The Main Main Menu Menu .............. .................... ............. .............. ............. ............. ............. ............. ............. ............. .............. ............. ............. ............. ............. ............. ........... ..... 61 Library Library Menu Menu ................. ........................ ............. ............. .............. ............. ............. ............. ............. .............. .............. .............. .............. ............. ............ ............. .......... ... 62 6.4.1 Sample Sample Menu .............. ..................... .............. ............. ............. ............. ............. .............. .............. .............. .............. ............. ............. ............. ......... ... 63 Review ............... ...................... ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............ ............ ............ ..... 69 6.5.1 6.5.1 Review Review - Displa Displayed yed Diagram Diagrams s ...... .......... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ...... .. 70 Setting Setting Up the Instrument Instrument .............. ..................... ............. ............. ............. ............. .............. ............. ............. ............. ............. ............. ............. ............. ........ .. 74

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6.6.1 Configuratio Configuration n ............. .................... ............. ............. .............. ............. ............. ............. ............. .............. ............. ............. ............. ............. ............. ...... 75 6.6.2 Printer Printer Setup ............. .................... ............. ............. ............. ............. ............. ............. ............. ............. .............. .............. ............. ............. ............. ...... 76 6.6.3 Serial Port Setup ............. .................... ............. ............. .............. ............. ............. ............. ............. ............. ............. .............. .............. ............. ...... 78 6.6.4 Safety Cooling Cooling .............. ..................... .............. ............. ............. ............. ............. .............. .............. ............. ............. ............. ............. ............. ......... ... 79 6.6.5 Rotors ............. ................... ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. .............. ............ ..... 80 6.6.6 Sensors Sensors ............ ................... ............. ............. .............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ......... ... 81 6.6.7 Accessories Accessories ............. ................... ............. .............. ............. ............. ............. ............. ............. ............. ............. ............. .............. ............. ............. ......... .. 82 6.7 Service Service .............. .................... ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............ ............. ............. ...... 83 6.7.1 Software Software Update Update ............. .................... ............. ............. ............. ............. .............. ............. ............. ............. ............. .............. .............. .............. ....... 84 6.7.2 Power Calibration Calibration ............. .................... ............. ............. .............. ............. ............. .............. ............. ............. ............. ............. .............. ............ ..... 84 6.7.3 Power Check ............. .................... ............. ............. .............. ............. ............. ............. ............. .............. ............. ............. ............. ............. ............. ...... 85 6.7.4 6.7.4 Tempera emperatur ture e Senso Sensorr Calib Calibrat ration ion with with the the Calib Calibrat ration ion Access Accessory ory ...... ......... ....... ........ ....... ....... ...... .. 86 6.7.5 6.7.5 Tempera emperatur ture e Sensor Sensor Calibr Calibrati ation on with with the Calib Calibrat ration ion Unit Unit ....... .......... ...... ....... ....... ....... ........ ....... ...... ...... ... 94 6.7.6 6.7.6 Tempera emperatur ture e Senso Sensorr Check Check with with the the Calib Calibrat ration ion Access Accessory ory ...... .......... ........ ....... ...... ....... ....... ....... .... 109 6.7.7 6.7.7 Tempera emperatur ture e Sensor Sensor Check Check with the Calibrati Calibration on Unit ......... ............ ...... ....... ....... ...... ....... ....... ...... ....... ....... ....1 .110 10 6.7.8 Temperature emperature Sensor Sensor Settings Settings ............. ................... ............. ............. ............. .............. ............. ............. ............. ............. .............. .......1 112 6.7.9 6.7.9 IR Sensor Sensor Calib Calibrat ration ion with with the Calib Calibrat ration ion Acces Accessor sory y ....... .......... ...... ....... ....... ....... ....... ...... ....... ....... ...... .....1 ..114 14 6.7.10 IR Sensor Sensor Calibration Calibration with the Calibration Calibration Unit .............. ..................... .............. ............. ............. ............. ...........1 .....118 18 6.7.11 6.7.11 IR Sensor Sensor Check with the Calibration Calibration Accessory Accessory .............. ..................... .............. ............. ............. .............. ....... 122 6.7.12 IR Sensor Check with the Calibration Calibration Unit ................... ......................... ............. ............. ............. .............. ............. ...... 124 6.7.13 Solvent Solvent Sensor Sensor Settings Settings ............ ................... ............... .............. ............. ............. ............. .............. ............. ............. .............. ............. ...... 125 6.7.14 Exhaust Exhaust Unit Installati Installation on ........... ................. ............. .............. ............. ............. .............. ............. ............. .............. ............. ............. ......... .. 127 6.7.15 Library Library Maintenanc Maintenance e Tool .................. ......................... .............. ............. ............. ............. ............. .............. ............. ............. ............. ...... 127 6.7.16 Advanced Advanced Service Service Routines Routines ................. ........................ ............. ............. .............. ............. ............. .............. ............. ............. ......... .. 129 6.8 Info .................. ........................ ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ........... ............ .............. ....... 130 6.9 AP Softprint Softprint ......... ................ ............. ............. .............. .............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ....... 131 7 Troub les ho ot in g ............... ..................... ............. ............. ............ ............. ............. ............. ............. ............. ............. ............ ............. ............. ............ ............. .............. ........... .... 132 7.1

Software Software ................ ....................... ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............ ............ ....... 132 7.1.1 7.1.1 Error Error Messag Message e Menu Menu - List of Erro Errorr Codes Codes ......... ............ ...... ...... ....... ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ....... ... 132 7.1.2 7.1.2 Pop-up Pop-up Error Error Mess Message ages s in the Case Case of an "Ala "Alarm" rm" ....... .......... ....... ....... ....... ....... ....... ....... ....... ....... ....... ....... ... 134 7.1.3 7.1.3 Pop-up Pop-up Messa Messages ges During During Syste System m Check Check ...... ......... ....... ....... ...... ....... ....... ....... ....... ....... ........ ....... ....... ....... ...... ....... ...... .. 138 7.1.4 7.1.4 Pop-up Pop-up Error Error Mess Message ages s During During Syste System m Check Check ....... ........... ....... ....... ....... ....... ....... ...... ....... ....... ....... ....... ...... ...... ... 139 7.1.5 7.1.5 Pop-up Pop-up Error Error Mess Message ages s Under Under Vari Various ous Cond Conditi itions ons ........ ........... ....... ....... ....... ....... ...... ....... ....... ...... ....... ....... ... 143 7.1.6 7.1.6 Pop-up Pop-up Erro Errorr Messa Messages ges Duri During ng "Powe "Powerr Calibr Calibrati ation" on" ........ ........... ....... ....... ....... ....... ...... ....... ........ ....... ...... ..... 147 7.1.7 7.1.7 Pop-up Pop-up Erro Errorr Messag Messages es Durin During g "Temp "Temp.. Senso Sensorr Calibr Calibrati ation" on" and and "Temp "Temp.. Sensor Sensor Check" ............................................................... .................................................. 149 7.2 Rotor 16 and and Rotor Rotor 8S ........ ............... ............. ............. .............. .............. ............. ............. ............. ............. .............. .............. .............. ............. ............. ......... .. 151 7.3 Sensors Sensors ................ ....................... ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............ ............ ....... 152 8 Roto r 48MF50 48MF50 .............. ..................... ............. ............. ............. ............. .............. .............. ............. ............. ............. ............. ............. ............. .............. ............. ............ ............. ....... 153 8.1 8.2

8.3 8.4

8.5

Technical echnical Descrip Description tion of Rotor Rotor 48 48 ............... ...................... ............. ............. ............. ............. .............. .............. .............. ............. ............. ............ ..... 153 8.1.1 8.1.1 Vessels essels for Rotor Rotor 48 ....... .......... ....... ....... ...... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ....... ...... ....... ...... .. 155 Limitatio Limitations ns of Operation Operation .............. ..................... ............. ............. .............. ............. ............. .............. ............. ............. ............. ............. .............. ............ ........ ... 156 8.2.1 Number Number of Vessels ............. .................... ............. ............. .............. ............. ............. .............. ............. ............. ............. ............. .............. ......... 156 8.2.2 Temperature emperature profiles profiles ............. .................... ............. ............. .............. ............. ............. .............. ............. ............. ............. ............. ............. ...... 157 8.2.3 Power Profiles Profiles ............. .................... ............. ............. .............. ............. ............. ............. ............. .............. ............. ............. .............. .............. ......... 157 8.2.4 Fan Settings Settings ............. .................... ............. ............. .............. ............. ............. ............. ............. ............. ............. ............. ............. .............. ............ ..... 157 Prior to the the First First Reactio Reaction n ............. ................... ............. ............. ............. ............. ............. .............. ............. ............. .............. ............. ............. ............. ........ 158 Performing Performing a Reactio Reaction n .................. ........................ ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ............. ........ .. 159 8.4.1 8.4.1 Adding Adding Reagen Reagents ts and Solvent Solvents s ....... .......... ....... ....... ....... ....... ...... ....... ....... ....... ....... ....... ....... ...... ....... ....... ....... ....... ...... ....... ....... ... 159 8.4.2 Closing Closing the Vessels Vessels ............. .................... .............. .............. ............. ............. ............. ............. .............. ............. ............. .............. ............. ...... 160 8.4.3 8.4.3 Loadin Loading g Rotor Rotor 48 ....... .......... ....... ........ ........ ........ ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ....... ...... ....... ....... ....... ...... 163 8.4.4 8.4.4 Perfor Performin ming g a Synthe Synthesis sis Run ....... .......... ....... ........ ........ ....... ....... ........ ....... ....... ....... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ... 165 8.4.5 8.4.5 Unload Unloading ing Rotor Rotor 48 ....... .......... ....... ....... ....... ....... ...... ...... ....... ....... ...... ....... ....... ...... ....... ........ ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ...... .. 167 Cleaning Cleaning and Maintenanc Maintenance e ................. ....................... ............. .............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ...... 170

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8.5.1 8.5.1 Cleani Cleaning ng of the Reactio Reaction n Vessels essels .......... .............. ....... ....... ........ ....... ....... ....... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ... 170 8.5.2 8.5.2 Cleani Cleaning ng After After Every Run ...... .......... ....... ...... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ....... ....... ...... 171 8.5.3 8.5.3 Checki Checking ng After Every Every Run ...... .......... ....... ...... ....... ....... ...... ....... ....... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ........ ....... ...... ....... ...... .. 174 8.5.4 8.5.4 Standard tandard Clea Cleanin ning g and Maint Maintena enance nce Proc Procedu edures res ......... ............. ........ ....... ...... ....... ....... ....... ....... ....... ....... ...... ... 175 8.5.5 8.5.5 Proced Procedure ures s After After the Rupture Rupture of a Safety Safety Disk Disk ....... .......... ....... ........ ....... ...... ....... ....... ....... ....... ....... ....... ....... ...... .. 179 8.5.6 8.5.6 Proced Procedure ures s After After a Vessel essel Explos Explosion ion ...... ......... ....... ........ ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ....... ........ ........ ....... ..... 185 8.6 Maintenance Maintenance of the Pressure Pressure / Temper Temperature ature Sensor Sensor M50 M50 ............. .................... .............. ............. ............. .............. .......... ... 195 8.6.1 8.6.1 Replac Replacing ing Seal Seal and Safety Safety Disk ....... ........... ....... ...... ...... ....... ....... ...... ...... ....... ....... ....... ....... ...... ....... ........ ....... ...... ....... ....... ...... ... 195 8.6.2 8.6.2 Replac Replacing ing the Thermom Thermometer eter Capill Capillary ary ....... .......... ...... ...... ....... ....... ...... ....... ........ ....... ...... ....... ....... ...... ...... ....... ....... ....... ...... 200 8.6.3 8.6.3 Replac Replacing ing the Immers Immersion ion Tube Tube ....... .......... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ...... .. 202 9 Roto r 16MF100 16MF100 / 16HF100 .............. .................... ............. .............. ............. ............. ............. ............. .............. ............. ............. ............. ............. ............. ............. ....... 205 9.1

Technical echnical Descrip Description tion of Rotor Rotor 16 16 ............... ...................... ............. ............. ............. ............. .............. .............. .............. ............. ............. ............ ..... 205 9.1.1 9.1.1 Vessels essels for Rotor Rotor 16 ....... .......... ....... ....... ...... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ........ ....... ...... ....... ....... ...... ....... ....... ....... ....... ..... 207 9.2 Prior to the the First First Reactio Reaction n ............. ................... ............. ............. ............. ............. ............. .............. .............. .............. .............. ............. ............. ............. ...... 209 9.2.1 9.2.1 To Prepar Prepare e the First First Run ....... .......... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ....... ....... ...... ....... ....... ...... ....... ....... ....... ....... ..... 209 9.3 Performing Performing a Synthesis Synthesis .............. .................... ............. ............. ............. ............. ............. ............. ............. .............. ............. ............. ............. ............. ........... .... 210 9.3.1 9.3.1 Adding Adding Reagen Reagents ts and Solvent Solvents s ....... .......... ....... ....... ....... ....... ...... ....... ....... ...... ....... ........ ....... ...... ....... ....... ....... ....... ...... ....... ....... ... 210 9.3.2 Assembling Assembling the Vessels .............. ..................... ............. ............. ............. ............. ............. ............. .............. ............. ............. ............. .......21 .211 1 9.3.3 9.3.3 Loadin Loading g Rotor Rotor 16 ....... .......... ...... ....... ....... ...... ...... ....... ....... ...... ....... ........ ....... ....... ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ....... ...... ...... ....... .... 220 9.3.4 9.3.4 Perfor Performin ming g a Synthe Synthesis sis Run ....... .......... ....... ....... ....... ....... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ...... .. 221 9.3.5 9.3.5 Unload Unloading ing Rotor Rotor 16 ....... .......... ....... ....... ....... ....... ...... ...... ....... ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ....... ...... ....... ........ ....... ...... ....... ...... .. 223 9.4 Cleaning Cleaning and Maintenanc Maintenance e ................. ....................... ............. .............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ...... 228 9.4.1 9.4.1 Cleani Cleaning ng of the Reactio Reaction n Vessels essels ......... ............. ....... ....... ........ ....... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ....... ....... ..... 228 9.4.2 9.4.2 Cleani Cleaning ng After After Every Every Run ...... .......... ....... ...... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ...... ....... ....... ...... ....... ....... ....... ...... 229 9.4.3 9.4.3 Checki Checking ng After Every Every Run ...... .......... ....... ...... ....... ....... ...... ....... ....... ....... ....... ...... ....... ....... ...... ....... ........ ....... ...... ....... ....... ...... ....... ...... .. 231 9.4.4 9.4.4 Standard tandard Clea Cleanin ning g and Maint Maintena enance nce Proc Procedu edures res ......... ............. ........ ....... ...... ....... ....... ....... ....... ....... ....... ...... ... 234 9.4.5 9.4.5 Proced Procedure ures s After After the the Breaka Breakage ge of a Safe Safety ty Disk Disk .......... ............. ....... ....... ...... ....... ....... ....... ....... ....... ....... ....... ...... 244 9.4.6 9.4.6 Proced Procedure ures s After After a Vessel essel Explos Explosion ion ...... ......... ....... ........ ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ....... ...... .. 247 9.4.7 9.4.7 Intens Intensive ive Cleani Cleaning ng of Ceramic Ceramic Vesse Vessels ls ....... .......... ...... ....... ....... ...... ....... ....... ...... ...... ....... ....... ...... ...... ....... ....... ...... ....... .... 253 9.5 Maintenance Maintenance of the the Pressur Pressure e / Temperature emperature Sensor Sensor Accesso Accessory ry ......... ............... ............. .............. .............. ............ ..... 255 9.5.1 9.5.1 Replac Replacing ing Seal Seal and Safety Safety Disk ....... ........... ....... ...... ...... ....... ....... ...... ...... ....... ....... ....... ....... ...... ...... ....... ....... ...... ....... ....... ...... ..... 255 9.5.2 9.5.2 Replac Replacing ing the Thermom Thermometer eter Capill Capillary ary ....... .......... ...... ...... ....... ....... ...... ....... ........ ....... ...... ....... ....... ...... ...... ....... ....... ....... ...... 260 9.5.3 9.5.3 Replac Replacing ing the Immers Immersion ion Tube Tube ....... .......... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ....... ...... ....... ...... .. 263 10 Roto r 8SXF100 / 8SXQ80 ............ .................... .............. ............. .............. ............. ............. .............. ............. ............. .............. ............. ............. .............. ............ ........ ... 265 10.1 Technical echnical Description Description of Rotor 8S ............. ................... ............. ............. ............. .............. ............. ............. ............. ............. ............. ............. ......... .. 265 10.1.1 10.1.1 Vessels essels for for Rotor Rotor 8S 8S ......... ................ ............. ............. .............. .............. ............. ............. ............. ............. .............. ............. ............. .......... ... 267 10.2 Prior to the First Reaction Reaction .............. ..................... .............. .............. ............. ............. ............. ............. ............. ............. ............. ............. .............. ............ ..... 270 10.2.1 10.2.1 To Prepare Prepare the First Run .............. .................... ............. .............. .............. ............. ............. .............. .............. .............. ............. .......... .... 270 10.3 Performing Performing a Synthesis Synthesis ............. .................... ............. ............. ............. ............. .............. ............. ............. .............. ............. ............. .............. .............. .......... ... 271 10.3.1 Adding Adding Reagents Reagents and Solvents Solvents ............ ................... .............. .............. ............. ............. .............. .............. .............. .............. ......... 271 10.3.2 Assembling Assembling the Vessels ............... ...................... .............. ............. ............. ............. ............. ............. ............. ............. ............. ............ ..... 272 10.3.3 10.3.3 Loading Loading Rotor 8S .................. ........................ ............. .............. ............. ............. .............. ............. ............. .............. ............. ............. ............ ..... 281 10.3.4 10.3.4 Performing Performing a Synthesis Synthesis Run ............. .................... .............. .............. .............. ............. ............. .............. ............. ............. ............. ...... 285 10.3.5 Unloading Unloading Rotor 8S ............. ................... ............. ............. ............. ............. ............. .............. ............. ............. ............. ............. .............. ......... 287 10.4 Cleaning Cleaning and Maintenanc Maintenance e ............. .................... ............. ............. .............. ............. ............. .............. .............. ............. ............. .............. ............. .......... .... 294 10.4.1 10.4.1 Cleaning Cleaning of the Reaction Reaction Vessels Vessels ............. .................... .............. .............. ............. ............. .............. ............. .............. ............ .... 294 10.4.2 Cleaning Cleaning After Every Run ........... .................. .............. .............. ............. ............. ............. ............. ............. ............. ............. ............. ....... 295 10.4.3 Checking Checking After After Every Run ............... ...................... ............. ............. ............. ............. .............. .............. .............. .............. .............. ....... 297 10.4.4 Standard Standard Cleaning Cleaning and Maintenanc Maintenance e Procedures Procedures ....... .............. .............. .............. ............. ............. ............. ...... 300 10.4.5 Procedures Procedures After After the Rupture Rupture of a Safety Disk ............. .................... ............. ............. .............. .............. ........... .... 312 10.4.6 Procedures Procedures After a Vessel Explosion Explosion .................... .......................... ............. ............. ............. .............. .............. ............. ...... 316 10.4.7 Intensive Intensive Cleaning Cleaning of Ceramic Ceramic Vessels ............ ................... ............. ............. ............. ............. ............. ............. ............ ..... 323 10.5 Maintenance Maintenance of of the T-Probe T-Probe and and the Immersio Immersion n Tube Tube with with Seal XF XF / XQ .............. .................... ............ ...... 324 10.5.1 Replacing Replacing the Seal and Safety Disk ............. .................... .............. .............. ............. ............. ............. ............. .............. ......... 324

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10.5.2 Replacing Replacing the Thermometer Thermometer Capillary Capillary ........ .............. ............. ............. ............. ............. ............. ............. ............. ............ ..... 328 11 Ap pl ic atio ns ............. .................... .............. .............. .............. ............. ............. ............. ............. ............. ............. ............. ............. .............. .............. ............ ............ .............. ......... .. 332 11.1 General General Information Information .............. ..................... .............. ............. ............. ............. ............. .............. ............. ............. ............. ............. ............. ............. ............. ........ .. 332 11.1.1 Basics Basics of Microwave Microwave Heating Heating .................. ........................ ............. .............. .............. ............. ............. .............. ............. ............. ....... 333 11.1.2 Hazards Hazards During During Microwave Microwave Synthesis Synthesis ............. .................... .............. ............. ............. .............. ............. .............. ............ .... 335 11.1.3 Reagents Reagents ............. .................... ............. ............. ............. ............. .............. .............. .............. .............. ............. ............. ............. ............. .............. ......... .. 338 11.2 Performing Performing Synthesis Synthesis .............. ..................... .............. ............. ............. ............. ............. .............. ............. ............. ............. ............. ............. ............. ............. ...... 347 11.2.1 General General ............. ................... ............. .............. ............. ............. ............. ............. .............. .............. ............. ............. .............. .............. .............. ............ ..... 347 11.2.2 Operation Operation Without Without an Internal Internal Temperature emperature Sensor Sensor ............. .................... .............. ............. ............. ........... .... 348 11.2.3 Operating Operating With Sensors Sensors ............... ...................... .............. ............. ............. .............. .............. ............. ............. ............. ............. ........... .... 348 11.2.4 Interpretati Interpretation on of Results Results ................ ....................... ............. .............. ............... .............. ............. ............. .............. ............. ............. ......... .. 351 11.2.5 Power Reduction Reduction by the Instrument Instrument .................. ........................ ............. .............. .............. ............. ............. .............. ......... .. 351 12 Ap pend ix ............. .................... .............. ............. ............. ............. ............. ............. ............. .............. ............. ............. ............. ............. .............. .............. ............ ............ .............. ......... .. 353 12.1 Addresses Addresses .............. ..................... ............. ............. .............. ............. ............. ............. ............. .............. .............. .............. .............. ............. ............. ............ ............ .......... ... 353 12.2 Packing Packing the Synthos Synthos 3000 and and the Rotors Rotors ............. .................... .............. .............. ............. ............. .............. .............. ............. ............ ...... 354 12.2.1 Packing Packing the Instrument Instrument .............. ..................... ............. ............. ............. ............. .............. ............. ............. ............. ............. .............. ......... 354 12.2.2 Packing Packing the Rotors Rotors .............. ..................... .............. .............. ............. ............. ............. ............. ............. ............. .............. ............. ............. ....... 358 12.3 Technical echnical Data of the Instrument Instrument ............. .................... .............. ............. ............. .............. ............. ............. .............. .............. .............. ............. ........ 360 12.3.1 12.3.1 Synthos Synthos 3000 Microwave Microwave Oven ............. .................... .............. ............. ............. .............. .............. ............. ............. .............. ......... 360 12.3.2 12.3.2 Options Options .............. .................... ............. ............. ............. .............. .............. ............. ............. .............. .............. ............. ............. .............. ............. ........... ..... 362 12.3.3 Rotor 48MF50 48MF50 ............. .................... .............. .............. ............. ............. ............. ............. .............. ............. ............. ............. ............. .............. ......... 362 12.3.4 12.3.4 Rotor 16 MF100 MF100 ............. .................... ............. ............. .............. ............. ............. .............. ............. ............. .............. ............. ............. ............ ..... 363 12.3.5 12.3.5 Rotor 16 HF100 .............. ..................... ............. ............. ............. ............. .............. ............. ............. ............. ............. .............. ............. ............ ...... 363 12.3.6 Rotor 8SXF100 8SXF100 ............. .................... ............. ............. ............. ............. ............. ............. ............. ............. .............. ............. ............. ............. ........ .. 364 12.3.7 12.3.7 Rotor 8SXQ80 8SXQ80 ........ ............... .............. .............. ............. ............. .............. ............. ............. .............. .............. .............. ............. ............. ............ ..... 364 12.4 List of Spare Spare Parts ............. .................... ............. ............. ............. ............. .............. .............. .............. .............. .............. .............. ............. ............. ............ ......... .... 365 12.5 Safety Certificat Certification ion ............. .................... ............. ............. .............. .............. .............. .............. ............. ............. ............. ............. .............. .............. ............. ......... ... 366 12.6 CE Declaration Declaration of Conformity Conformity ............. .................... ............. ............. .............. .............. ............. ............. .............. ............. ............. .............. ............. ...... 368 12.7 Safety Declaration Declaration for for Repair Repair and Malfuncti Malfunction on Report Report .............. ..................... ............. ............. .............. .............. .............. ....... 369

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1 Introduction

1 In t r o d u c t i o n

Synthos 3000 is a scale-up-instrument for microwave-assisted chemical synthesis. It has different rotors for various fields of application in organic synthesis chemistry employing closed vessels. Powerful microwave generators (magnetrons) allow efficient heating of large amounts of solvents.

Fig. 1 - 1

Synthos 3000

Parallel rotors with up to 48 positions can be used to carry out temperaturedependent processes in the microwave field, saving time. A specially designed rotor with robust quartz glass vessels enables reactions under extreme pressure and temperature conditions which are difficult to reach safely with conventional systems. The components are highly compatible with each other, making the system suitable for a variety of different applications.

Syntho s 3000 excels in:

• • • • •

Easy oper peration Excell Excellent ent reprodu reproducib cibili ility ty of result results s Direct Direct scala scalabil bility ity of react reaction ion proto protocol cols s up to the lite literr scale scale Maximu Maximum m safet safety y unde underr extre extreme me condit condition ions s Effect Effective ive scal scale-up e-up and high high samp sample le throu throughp ghput ut

This makes Synthos 3000 a high-performance instrument for the production of numerous compounds in pharmaceutical, biomedical and other organic-chemical synthesis laboratories. Synthos 3000 has been developed by Anton Paar GmbH as a result of its longstanding experience and in close cooperation with the Karl-Franzens University in Graz, Austria.

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2 Symbols

2 Symbols 2.1

Symbols in the Instruction Manual

Warning: The "Warning" sign indicates a hazard . It calls attention to an operating procedure, practice, etc. which could result in injury or loss of life, if not correctly performed or adhered to. Do not proceed beyond a "Warning" sign until the indicated conditions are fully understood and met.

Important: The "Important" sign indicates a hazard . It calls attention to an operating procedure, practice, etc. which could result in damage or destruction of the instrument or parts of it, if not correctly performed or adhered to. Do not proceed beyond an "Important" sign until the indicated conditions are fully understood and met.

Hint: The "Hint" sign calls attention to additional information, which might be

useful to the operator.

2.2

Safety Symbols Applied to the Instrument

Warning screen located on the front door of the instrument.

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2 Symbols

Warning screens located on the front side and on the right side panel of the instrument.

Symbol located on the rotors: Refer to the manual!

Warning screen located on Rotor 48.

Symbol located on the calibration accessory: Caution - hot surf ace!

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3 Safety Instructions

3 Safety Instructions Synthos 3000 has been tested and is listed for compliance with US, Canadian and European standards by Intertek Testing Services, which is an accredited testing lab. The instrument was found to be fully compliant with the Equipment Safety Law. This indicates the high safety standard of the Synthos 3000 system. Hint: This instruction manual is supplied with Synthos 3000 and contains important information and warnings that must be followed by the user to ensure safe

operation and to maintain the instrument in safe condition. This manual is intended to supplement, not supersede, the normal safety code of conduct of each individual country of operation. The provided information does not cover every safety procedure that should be practiced. Ultimately, the operator's organization bears responsibility for the adherence to safety rules. Possible hazards that could harm the user or result in damage to the instrument are clearly stated at appropriate places throughout this instruction manual as well as in the reference manual.

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3.1

General Safety Instructions for Synthos 3000

Important: Read this reference manual carefully before the first use of your instrument! Make sure that all instructions are fully understood and met to ensure safe and efficient operation of Synthos 3000.

Warning: The instrument cavity is equipped with light emitting diodes (LED). Do not look directly into the light with optical instruments as the LEDs are class 1M laser products.

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All operators have to be sufficiently trained in the correct and safe use of this instrument. Operators must be able to judge dangerous situations and take the right measures to prevent accidents, injuries and damages.

•

The operation of the pressure vessels may be liable to individual national regulations. The operator is responsible for the correct installation, handling and service of the pressure vessels and for sufficient training of the operating staff.

•

Do not use Synthos 3000 for any purpose other than described in this instruction manual or the reference manual, respectively. Anton Paar GmbH accepts no responsibility for injuries or damages caused by unauthorized use of the instrument.

•

Follow the installation instructions provided with this manual. The installation has to be carried out by qualified personnel who ar e able to read, understand and apply these instructions.

•

This instrument is not designed for operation in an explosive atmosphere.

•

Synthos 3000 is equipped with strong permanent magnets. Keep the following items away from Synthos 3000: credit cards and other cards with a

9


magnetic read-write band, pacemakers or similar items, magnetic storage media such as floppy disks, DAT, ZIP, video cassettes, as they might be damaged by the permanent magnets. •

Do not lift or carry the instrument by its door. Warning: Do not lean against the instrument or the door, respectively. In case of a sudden pressure build-up inside the cavity (opening of a safety disk, vessel breakage) the door will slightly open for less than a second and noxious reaction gases may be released.

Warning: This instrument features strong magnets to close the door. People with pacemakers should kee p a distance of at least 50 cm to the instrument. During operation (microwave energy "ON") an electromagnetic field is generated by two transformers. Keep a safe distance of approx. 1 m to ensure maximum safety.

•

Under adverse conditions chemical syntheses may lead to violent, spontaneous reactions in which gaseous reaction products and solvent vapors may escape. Thus, the Synthos 3000 has to be installed in a fume hood.

•

The hood must be closed immediately after starting an experiment.

•

Do not to store containers with flammable reagents or other ignitable materials (e.g. soaked cleaning paper) close to the instrument.

•

Indoor use only!

•

Synthos 3000 should be supervised at all times during operation. Warning: - Never open the door during a running program! - If you abort a reaction procedure, wait until the safety cooling has been automatically stopped, i.e. the vessel temperatures are lower than the above mentioned limits. - After a mains power failure, wait for the vessels to cool down sufficiently before taking the rotor out. If a failure does not allow you to activate the safety cooling, it may take up to six hours for the vessels to cool down!

•

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In case of a safety disk breakage turn off the instrument after the cooling has been finished, and remove the rotor. Clean the instrument and rotor parts carefully and inspect them for visual damage. If the door shows deformations or can no longer be closed tightly, an increased risk of microwave radiation

10


leakage may consist. Do not continue to operate Synthos 3000 unless an authorized service engineer has checked the instrument for microwave radiation leakage. •

Never clean the rotor body and lid with organic solvents, especially halogenated hydrocarbons or acetone.

•

Never leave a rotor inside the Synthos 3000 oven when transporting the instrument. This could damage the microwave cavity or the door. Warning: Do not open the instrument casing, as this would uncover live parts. Repair

work has to be carried out by authorized field service engineers or by Anton Paar GmbH only.

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Anton Paar GmbH warrants proper function and safe operation only if no unauthorized modifications have been made to mechanical or electronic parts or software.

•

When passing this instrument to other users, also hand over all documentation and manuals.

11


3.2 •

Safety Instructions for Chemical Synthesis

Synthos 3000 is a scale-up instrument for use with optimized microwave protocols. Using the instrument to develop new methods requires special caution.

Warning: Always wear goggles, protective gloves and appropriate protective clothing when handling chemical reagents. Follow any special national safety regulations.

•

When performing a new synthesis for the first time, begin with small amounts and diluted solutions.

•

Never carry out syntheses in open vessels in the Synthos 3000. Warning: Do not use any sensors, accessories or consumption parts other than those supplied by Anton Paar GmbH, as this might result in serious damage to the

instrument or injuries of users.

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Never operate Synthos 3000 without sufficient load. Never use less than 4 vessels, as surplus microwave energy may interact with rotor parts and damage them.

•

Do not mark plastic parts of pressure vessels or rotors of microwave systems with pencils or markers containing conductive ink. A line of electrically conductive substance on the surface of a plastic part may interact with the microwave field, leading to local overheating of the plastic material up to destruction of rotors.

•

Make sure to apply reaction mixtures with adequate coupling efficiency. If you use materials with poor microwave absorption properties, we recommend using special heating elements.

•

Allow the vessels to cool down to a vessel interior temperature below 60 °C and to a vessel surface temperature (IR) below 50 °C before removing the rotor. Hot and pressurized vessels are dangerous if removed from the instrument.

•

Vent the reaction vessels either inside the microwave cavity of Synthos 3000 with the exhaust unit activated or under a working fume hood. Noxious gaseous reaction products may be released.

•

Do not operate Synthos 3000 if a fault is suspected.

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If there is a fault (e.g. opening of the safety disk) let the safety cooling run for at least one hour then switch of the instrument. Refer to the reference manual. Clean the instrument carefully and inspect it for visible damage. If the door can no longer be closed tightly, there is a danger of increased microwave radiation. Do not continue operating Synthos 3000.

•

After a (very unlikely) explosion of a vessel, do not continue with synthesis reactions. A service engineer has to perform an inspection and microwave leakage test.

13


3.3

Unexpected Operation Behavior

Synthos 3000 has been designed for safe operation even in case of incidents. In case of safety disk- or vessel breakage, the microwave power is shut down immediately due to the sudden overpressure release inside the cavity and the safety door opening. Normally, the safety cooling is activated simultaneously. Let the safety cooling run for at least one hour, then switch off the instrument and proceed as described in the reference manual. Although highly unlikely, it is still possible that a reaction procedure is terminated in an abnormal way due to an instrument failure. In such a case it is vital to act properly, thus strictly adhering to the instructions below. Warning: In case of unexpected operation behavior, NEVER open the door of Synthos 3000! Hot and pressurized vessels inside! The opening of the door will deactivate a vital safety feature, which is indispensable to ensure user safety. Af ter a po wer fai lu re:

•

Switch on the instrument again. If the safety cooling does not start automatically, gently pull the door (Fig. 3 - 1). The door will still be held by its safety hooks, while the door switches will trigger the safety cooling. Do not use the door opener! Switch off the instrument after one hour of safety cooling, as the cooling will not stop automatically.

Fig. 3 - 1

•

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Manual activation of safety ccoling

If the instrument cannot be switched on again, wait for the vessels to cool down. Depending on the reached temperature, the type of vessels as well as the number and loading of the vessels, it may take up to six hours for the vessels to cool down! Do not open the door earlier than after these six hour s!

14


Warning: Before removing a rotor from a switched off instrument, make sure that rotor and vessels have been cooled down completely! To do so, you can switch on

the instrument and check if the last run was finished completely (Review menu). If you are not sure whether rotor and vessels have cooled down, wait at least six hours before removing the rotor. Af ter an ex hau st un it fai lu re:

•

Wait for the vessels to cool down. If the exhaust unit fails during the run, terminate the run by pressing the button twice. Depending on the reached temperature, the type of vessels as well as the number and loading of the vessels, it may take up to six hours for the vessels to cool down! Do not open the door earlier than after these six hours !

Af ter a sy st em f ail ur e:

•

In very rare cases the instrument might reset during a run. After the automatic restart the safety cooling is usually activated by default. If the safety cooling does not start automatically, gently pull the door (Fig. 3 - 1). The door will still be held by its safety hooks, while the door switches will trigger the safety cooling. Do not use the door opener! Switch off the instrument after one hour of safety cooling, as the cooling will not stop automatically.

•

If the safety cooling can not be started, wait for the vessels to cool down. Depending on the reached temperature, the type of vessels as well as number and loading of the vessels, it may take up to six hours for the vessels to cool down! Do not open the doo r earlier than after these six hou rs!

In case of fir e inside the microwave cavity:

•

Switch off the instrument. Never open the door to extingui sh the fire! The emitted flue gas will cause the fire to die out rapidly. Thus do not activate the safety cooling! Warning: Hot pressure vessels! Overheating may result in rupture of safety disks or vessels! The design of the

oven cavity ensures user safety even in case of unexpected operation behavior. This safeguard is only provided if the door is kept shut!

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As a precaution keep a fire extinguisher ready or call for corresponding assistance.

•

Due to the possibility of escaping fumes it is recommended to switch on the fume hood(s) and to leave the lab. Look after the instrument temporarily.

15


•

After the fire is extinguished wait at least six ho urs before opening the door. Waiting six hours ensures that rotor and vessels are cooled down sufficiently and overpressure is diminished.

Important: Always check rotor and vessels carefully for damage if a run has been interrupted unexpectedly.

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4 Technical Description of Synthos 3000


The following chapters contain a short description of the working principle, fields of application and the technical description of the instrument as well as of available sensor accessories.

4.1

Working Principle

The reagents are weighed into the reaction vessels made of quartz or fluoropolymers. The vessels are closed by a screw cap (Rotor 16 and Rotor 48) or by a seal holder (Rotor 8S). The vessels are sealed either with a self-sealing lip-type seal (Rotor 8S and Rotor 16) or a conical seal (Rotor 48). The pressure vessels are inserted into the rotor, the closed rotor is placed into the Synthos 3000 oven and the door is closed. A built-in microcontroller controls the reaction processes, stores a method library and documents the reaction process. Depending on the rotor type and accessories used, the operating pressure and temperature can be recorded simultaneously and displayed. The measured data is transmitted wireless from the rotor to the built-in microprocessor. As soon as one of the predefined limits is reached, the microwave energy is reduced or completely switched off. If necessary, cooling intensity is increased. In addition the surface temperature of the reaction vessels is measured using an infrared sensor. During the process, the integrated cooling system generates a slight cooling air flow along reaction vessels and therefore protects rotor components against excessive thermal stress of rotor and vessels. This has a positive effect on the service life of the components.

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4.2

Fields of Application

The main field of application for Synthos 3000 is the synthesis of organic compounds in the pharmaceutical, biomedical and agrochemical industry in the 50-250 g range using optimized methods. The numerous accessories for Synthos 3000 also make it ideal for special applications such as reactions under different atmospheres, extreme pressure and temperature conditions and for carrying out cleaning and processes steps. Compared with other microwave synthesis systems, Synthos 3000 provides the highest safety standards, high quality accessories and excellent reproducibility of the experiments. This is due to: •

unpulsed continuously adjustable microwave energy over the whole power range

•

direct scalability, from milliliters to liters without changing the reaction parameters

•

the highest available pressure and temperature limits

•

innovative and practical rotor and vessel design

•

efficient vessel cooling

•

easy-to-operate program functions.

As well as conventional microwave-assisted synthesis, the following applications can also be carried out:

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Reactions under pressure with individually applied reactant or inert gas atmosphere

•

Efficient high-temperature synthesis with low absorbing solvents utilizing silicon carbide (SiC) heating elements

•

Near critical water chemistry

•

Protein hydrolysis

•

Solid phase synthesis including cleavage and filtration in the same vessel

18


4.3

Technical Description of the Instrument

The microwave cavity is sealed by a safety door, which can be opened easily by pressing the door opener button. Above the door is a graphic display and an acid- and water-repellent keypad. To the right of the keypad is space to place the alphanumeric keyboard. The main switch for the instrument is located at the front lower right corner of the instrument.

Graphic display

Keypad foil



Door opener (not visible)

button

Space for the alphanumeric keyboard

Door

Mains switch

Fig. 4 - 1

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Front view of Synthos 3000

19


Turntable

Fig. 4 - 2

View into the opened microwave cavity (without rotor on the left, with rotor on the right)

Exhaust unit

Fitting for exhaust hose Electrical supply of the exhaust unit

Mains supply

Fig. 4 - 3

Rear side of Synthos 3000, view of the exhaust unit

The exhaust unit and the appropriate electrical connections are located on the rear side of the instrument together with the mains supply socket. Ports for optional accessories, interfaces and the view angle control knob for the graphic display are located on the right side of the instrument:

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3

1

2 Fig. 4 - 4

1

4

5

6

7

Electrical connections/ports on the right side of Synthos 3000

Serial RS 232C int erface (COM1) This port is used to connect Synthos 3000 to the serial (RS 232C) interface of a PC via a serial link cable (0-Modem

cable, Mat.No. 70429). For computer with USB-port only an USB to RS232 converter cable (Mat.No. 17562) is needed. 2

Serial RS 232C interface (COM2)

This port is for maintenance purpose only. 3

View angle con trol for t he graphic d isplay (VIEW ANGLE) Use this knob to adjust the view angle of the graphic display (LCD).

4

External alphanumeric keyboard (KEYB) This port can be used to connect the alphanumeric keyboard.

5

Calibratio n port (CAL) The temperature sensor accessories must be calibrated from time to time. Use this port to connect the temperature calibration accessory for calibration of the sensor accessories.

6

Au xi li ary po rt fo r o ptio nal acc ess or y (A UX) This port can be used to connect auxiliary/optional accessories (e.g. solvent sensor).

7

PRINTER

Parallel (Centronics) interface to connect printers.

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4.3.1

Mi cr ow av e Heat in g

Microwave radiation is an electromagnetic radiation in the frequency range from 300 MHz to 300 GHz. Synthos 3000 comes with two microwave generators (magnetrons) that generate microwave radiation at a frequency of 2.45 GHz. Materials exposed to microwave radiation will react differently depending on their dielectric constants. They may reflect the microwaves (e.g. metals) or allow the permeation of radiation without being heated up (e.g. glass or plastics). Other substances, i.e. water, can absorb microwave energy, whereas polar molecules are stimulated to oscillate and dissolved ions can be moved through the electromagnetic field. Both effects cause the substance to heat up. These properties are the key to fast and efficient heating time of aqueous solutions and other polar substances. In contrast to the conventional heating in heating blocks or ovens (where the heat has to be transferred to the medium via metal parts, air or vessels), microwave radiation heats up the medium directly, which results in significant saving of time in many fields of application.

4.3.2

Mag net ro n Pr ot ec ti on

In order to prevent damage of the magnetrons by reflected power and to i ncrease the service life of magnetrons, several features are installed in the instrument: • • • •

Optimized waveguides for minimum reflected power Magnetron core temperature control Magnetron thermoswitch Soft start electronics

4.3.3

Unpulsed Energy Control

The unpulsed ("continuous") energy control contributes significantly to the synthesis quality and operational safety of the system.

Fig. 4 - 5

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Comparison of pulsed and unpulsed energy control

22


Energy supply of conventional microwave instruments usually applies maximum power in various duty cycles only. As a consequence, even at low power levels samples are irradiated with maximum power, thus making it difficult to control critical reactions. Synthos 3000 supplies unpulsed microwave energy over the entire power range.

This brings the following benefits: •

Uniform heating properties

•

Enhanced reaction control

•

Prevention of spontaneous reactions

•

Shorter reaction times

4.3.4

Saf et y Feat ur es

The pressure / temperature (p/T) monitoring and unpulsed microwave energy control ensure a high degree of operational safety. To ensure maximum protection in the case of spontaneous reactions, Synthos 3000 has been equipped with additional safety features.

Safety features:

• • • • • •

•

Monitoring of the pressure increase rate Built-in metal safety disks Use of special vessel jackets Effective rotor design Special construction of the instrument door Effective safety cooling

Monitoring of the pressure increase rate

If a p/T sensor accessory (optional) or Rotor 8S is used, the pressure increase rate can be limited to 0.1 - 3.0 bar/sec. By reducing the limit of the pressure increase rate, spontaneous reactions can be controlled very quickly by automatically reducing the microwave power in an early stage of the reaction. A possible rupture of the safety disk can be prevented in most cases.

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In addition, the sensor unit includes a second electronic protection circuit that reacts as soon as the maximum pressure increase rate of 3.0 bar/s is exceeded. In this case, microwave power is completely shut down (temporarily) and safety cooling is activated.

•

Built -in metal safety disks

Each pressure vessel is protected by a metal safety disk. If the pressure exceeds the permitted pressure limit (due to spontaneous chemical reactions or thermal runaways), the safety disk breaks and the pressure is released. This usually prevents the pressure vessels from rupture.

Safety disk Safety disk holder

Screw cap

Fig. 4 - 6

•

Screw cap (Rotor 16), safety disk and safety disk holder

Use of special vessel j ackets

The vessel jacket serves as a mechanical protection. Depending on the required pressure stability, the vessel jacket is either made of PEEK (for operating pressures up to 20 bar) or ceramics (for operating pressures up to 60 bar). The quartz glass vessels for Rotor 8S (for operating pressures up to 80 bar) are vessel jacket as well as reaction vessels; they are inserted directly into the protective casing.

•

Effective rotor design

The rotor surrounds the vessels and has been designed to ensure that the microwave cavity is well protected in the case of safety disk or vessel rupture.

•

Special construction o f the instrument door

The instrument door is locked by means of a mechanical interlock. To unlock and open the door, press the door opener button at the top of the instrument cover.

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Fig. 4 - 7

Door opener button

Permanent magnets effectively support the opening and closing mechanism of the door. The instrument door is equipped with two strong saf ety hooks that allow the door to open only a little slit. In the case of overpressure in the microwave cavity the door is opened slightly to release the overpressure and immediately closed by the magnets.

Safety hooks

Fig. 4 - 8 •

Instrument door with safety hooks

Ef fec ti ve saf et y co ol in g

The safety cooling cools down the hot, pressurized vessels and exhausts any reaction products that have escaped after the rupture of a safety disk or vessel. The safety cooling system is activated:

• • • •

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after termination of a program when starting up Synthos 3000 again after an interrupted reaction program (e.g. due to a power failure) if the pressure increase rate has exceeded 3.0 bar/s if no cooling step has been programmed

25


•

Temperature sensor "magnetron"

Temperature sensors are assembled on each of the two magnetrons (microwave generators). If overheating occurs, the magnetrons are shut down.

•

Temperature sensor " exhaust unit"

This temperature sensor is directly built into the exhaust unit and protects it against thermal overload.

•

Temperature sensor " exhaust air"

This sensor detects the temperature of the exhaust air. If the temperature of the exhaust air exceeds 130°C both microwave energy and cooling are switched off and a fire alarm is shown on the display.

4.3.5

Co ol in g an d Ex hau st

Synthos 3000 includes an "exhaust unit" that is programmable in four intensity steps and permanently carries off the reaction heat during the reaction in order to reduce the thermal stress on the used materials. Due to the permanent cooling during the process, a temperature gradient is built up in the vessel which leads to strong convection behavior and constant exchange between the liquid and the gaseous phase. Any gases which may escape during the reaction are withdrawn by the exhaust system. After completion of reaction the vessels are automatically cooled down below an appropriate temperature limit.

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Fig. 4 - 9

4.3.6

Integrated cooling unit

Ro to r Det ec ti on

Modern sensor technologies are an indispensable part of powerful, innovative instruments, such as Synthos 3000. The more accurate information about physical parameters is provided, the more successful demanding technical processes can be controlled. A wide range of additional sensors is available for improved, reliable results and higher operational safety. The standard version of Synthos 3000 includes optical sensors which are located in the microwave cavity of the instrument:

•

Position and protection lid recognition

A sensor located in the base of the oven cavity sends an infrared light beam onto the bottom plate of the rotor. The bottom plate reflects the beam to the sensor, which is electronically analyzed. The following information and/or functions are processed:

• Au to mat ic det ect io n o f t he r ot or ty pe This feature rules out errors caused by improper handling/operation. •

Monitoring the revolution of the rotor This feature monitors the rotor's revolution (RPM revolution per minute),

which is important for uniform microwave heating. Local overheating is avoided and the risk of spontaneous reactions is minimized.

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•

Exact position detection This function assigns the temperature measured by the IR sensor to each pressure vessel. In this way, the temperature course of each vessel can be followed and displayed.

•

Rotor lid detection

A sensor located on the right inner wall of the microwave cavity sends an infrared light beam to the rotor lid and (via a reflecting surface) back to the sensor. This function prevents an inadvertent start o f the reaction program without the rotor lid (which is an indispensable safety requirement).

Rotor lid detection

IR sensor

Position and rotor detection Fig. 4 - 10

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Rotor sensors

28


Reflecting surfaces

Light beam

Reflection

Rotor surface Microwave cavity

Sensor

Evaluation Electrical Signal

Fig. 4 - 11

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Working principle of the rotor sensors

29


4.4

Technical Description of the IR Temperature Sensor Ac cessory

The infrared sensor measures the temperature at the base surface of each reaction vessel. Measured temperature values are assigned and recorded to the corresponding vessel via the automatic position recognition. The temperature measurement protects against overheating. As the measurements are taken through a Fresnel lens on the bottom of the microwave cavity, make sure that this Fresnel lens is always kept clean.

Reaction vessel

IR radiation

Fresnel lens Electronic module

IR sensor

Fig. 4 - 12

IR temperature sensor - working principle

Temperature measuring range

20 - 400 °C

For checking and calibrating the IR sensor see Chapter 6.7.9 or Chapter 6.7.10 and Chapter 6.7.11 or Chapter 6.7.12. Important: The IR sensor has to be checked (and recalibrated, if necessary) at least once a year.

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4.5

Technical Description of the Pressure / Temperatur e Senso r Acc essory

This description applies for both, p/T sensor accessory for Rotor 16 and p/T sensor accessory M50 for Rotor 48. These tools are optional, but recommended to be used for optimum reaction control.

Electronics

Fig. 4 - 13

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Receiver

Knurled nut

Pressure / Temperature sensor - schematic description

31


Thermometer Capillary

Immersion Tube

Vent Pipe Seal Seal Husk

Fig. 4 - 14

Pressure/Temperature Sensor M50 (Rotor 48)

Gas bulb thermometer with capillary

PEEK protection tube

Syringe connector with O-ring

Venting screw

Immersion tube Seal holder Seal

Safety disk holder

Seal husk

Safety disk M&H Fig. 4 - 15

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Pressure / Temperature Sensor Accessory (Rotor 16)

32


4.5.1

Pressure Measurement

A hydraulic piston is installed in the sensor head above the seal of the reference vessel. This piston takes up the reaction pressure via the seal and the seal holder. The hydraulic system transfers the pressure of the reference vessel to the sensor module, where it is measured continuously during the reaction and transferred wireless (via IR) to the control electronics for the following purposes: •

Display and storage of the pressur e graph

The pressure of the reference vessel can be displayed on the graphic display during and after the reaction program (via the Review dialog). Values and graph can be printed out for documenting purposes or sent to an external PC after completion of the reaction run. •

Hardware monito ring of the pressure increase rate The sensor head of the p/T sensor accessory includes a special

microprocessor for software-independent monitoring of the pressure rate. As soon as the pressure increase rate reaches 3.0 bar/s or higher , the electronic module responds as follows: • •

• • •

Microwave generation will be completely shut down for a least 3 seconds. The cooling intensity of the exhaust unit will be increased temporarily to level 3; (for max. 120 seconds, or until the pressure rate shows a negative value for a defined period of time). After reaching normal pressure rate values the microwave power is gradually increased until it has reached the default value. A pop-up message informs the customer about the pressure increase rate.

Software-controlled pressure increase rate monitoring

During a reaction run, the software monitors the pressure increase rate in the vessel. As soon as the pressure increase rate limit (selectable in the method between 0.1 - 3.0 bar/s ) has been reached or exceeded the instrument responds as follows: • •

•

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If the pressure increase rate is 0.1 - 0.2 bar/s below the limit, the microwave power is reduced. If the pressure increase rate limit is reached, the microwave power will be cut off until the pressure rate is below the selected limit value; thereafter it will gradually increase again. If, after cutting off the microwave power, the pressure limit has NOT fallen below the limit value within 2 seconds, the intensity of the exhaust unit will be increased to its highest level (level 3).

33


•

Co nt ro l o f p res su re l im it

•

If the pressure exceeds the limit (20 bar fo r MF50 and HF100 and 40 bar for HF100) by more than 5 bar as a result of a spontaneous reaction, the experiment will be terminated. In this case the vessels and seals must be cleaned and checked very carefully for signs of damage.

Pressure measuring range

0-86 bar

Accuracy

± 0.2 bar

4.5.2

Temperature Measurement

Important: After (accidentally or on purpose) opening of the conical seal of the capillary tube (knurled nut on the pressure sensor unit), the temperature sensor has to be re-calibrated.

A hermetically sealed glass bulb is filled with gas. The gas in the bulb expands with increased temperature during the reaction. This gas expansion causes an increased pressure which is transferred to the pressure sensor via a capillary. The pressure increase is converted to a corresponding temperature value. This temperature value of the reference vessel is transmitted to the electronics module and from there wireless (via IR) to the microwave oven. The temperature is displayed graphically on the LCD as a “temperature over time” graph or as a numeric value. Using the optional calibration unit the immersion thermometer can be calibrated to an accuracy of ± 1% within a measuring range of 0 to 280°C. (Refer tochapter 6.7.4, "Temperature Sensor Calibration with the Calibration Accessory" or chapter 6.7.5, "Temperature Sensor Calibration with the Calibration Unit". Hint:

Calibration has to be done once a year, although it is recommended to calibrate the temperature sensor at least twice a year.

Each p/T Sensor Accessory is shipped with a unique serial number that is printe d on an adhesive label and stored in the sensor electronics. Synthos 3000 uses this information to identify the appropriate p/T Sensor Accessory and to assign the correct calibration factors.

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Control of temperature limit

•

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If the temperature exceeds the limit (200 °C fo r MF50, 190 °C fo r MF100 and 240 °C for HF100) by more than 5 °C as a result of a spontaneous reaction, the reaction run will be terminated. In this case the vessels and seals must be cleaned and checked very carefully for signs of damage.


0 - 280°C

Accuracy within a range of 0 - 200°C

± 1%

35


4.6

Technical Description of the T-Probe

Hint: The T-probe unit of Rotor 8S can be used for both pressure vessel types, XF100 and XQ80 and is used together with immersion tube with seal XF or

immersion tube with seal XQ. This optional accessory can be easily installed by the customer and it is recommended to use for optimum reaction control

Safety disk holder

Syringe connector with O-Ring

Safety disk X

Venting screw Seal XQ or XF Seal husk

Immersion tube

Knurled nut Fixing screw Capillary T-probe

Fig. 4 - 16

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T-probe S and corresponding immersion tube

36


4.6.1

Temperature Measurement

Important: After (accidentally or on purpose) opening of the conical seal of the capillary tube (knurled nut on the pressure sensor unit), the temperature sensor has to be re-calibrated.

A hermetically sealed glass bulb is filled with gas. The gas in the bulb expands with increased temperature during the reaction. This gas expansion causes an increased pressure, which is transferred to the pressure sensor via a capillary. The pressure increase is converted to a corresponding temperature value. This temperature value of the reference vessel is transmitted to the electronics module and from there wireless (via IR) to the microwave oven. The temperature is displayed graphically on the LCD as a “temperature over time” graph or as a numeric value. Using the optional calibration unit the immersion thermometer can be calibrated to an accuracy of ± 1% within a measuring ran ge of 0 to 300 °C. Refer tochapter 6.7.4, "Temperature Sensor Calibration with the Calibration Accessory" or chapter 6.7.5, "Temperature Sensor Calibration with the Calibration Unit".

Hint: Calibration has to be done once a year, although it is recommended to calibrate the temperature sensor at least twice a year.

Each T-probe accessory is shipped with a unique serial number that is printed on an adhesive label and stored in the sensor electronics. Synthos 3000 uses this information to identify the appropriate T-probe accessory and to assign the correct calibration factors. •

Control of temperature limit

•

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If the temperature exceeds the limit (260 °C for XF100 and 300 °C for XQ80) by more than 5 °C as a result of a spontaneous reaction, the reaction run will be terminated. In this case the vessels and seals must be cleaned and checked very carefully for signs of damage.


0 - 300°C

Accuracy within a range of 0 - 200°C

± 1%

37


4.7

Technical Description of the Safety Module SOLV

The safety module SOLV is a hardware accessory for Synthos 3000, which is mandatory for safe operation using organic solvents. It consists of mainly two membrane switches, which monitor the exhaust airflow through the cavity in order to prevent the formation of dangerous concentrations of solvent vapors inside the system. In case that the airflow is interrupted (e.g. failure of the exhaust fan, blocking of the exhaust system), microwave power is switched off immediately and the current run is interrupted. The safety module SOLV is installed underneath the cavity, therefore later upgrades in the field have to be done by authorized service engineers only.

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4.8

Technical Description of the Solvent Sensor Ac cessory

Fig. 4 - 17

Solvent sensor accessory

The optional solvent sensor monitors the concentration of organic solvents in the exhaust air channel of Synthos 3000. The sensor element is a metal oxide semiconductor detector that changes resistance in correlation to the gas concentration. The factory-calibrated Solvent Sensor Accessory is mounted instead of the cover on the exhaust channel at the rear side of the oven. It is electrically connected to the "AUX" port. Use the latest software version to monitor the solvent concentration and to trigger alarm functions, like increasing the speed of the exhaust fan. The solvent sensor is not required for instrumental safety. This is provided by the mandatory Safety Module SOLV.

4.8.1

Install ati on

Important: Take care that Synthos 3000 is switched off before installing the Solvent Sensor Accessory!

The Solvent Sensor Accessory measures the solvent concentration inside the cavity, but it is not required for safe use of the instrument like the obligatory Safety Module SOLV (SMS).

4.8.1.1

To Install the Solvent Sensor Accessory

1. Remove the safety bracket and the cover from the exhaust channel at the rear of Synthos 3000 by loosening the two nuts. 2. Plug the sensor into the exhaust channel. The cable has to point to the left.

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6 Software

Fig. 6 - 26

Temperature sensor calibration

3. Connect the cable of the calibration accessory to the CAL port on the righthand side of the instrument. Tighten the screws of the plug to ensure good contact.

Fig. 6 - 27

Connecting the cable of the calibration accessory to the instrument

4. Press the key to start the calibration. The serial number of the temperature sensor is read out first. The calibration accessory starts to heat and the temperature values are recorded automatically.



Fig. 6 - 28

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88

6 Software

5. At the end of the heating phase (approx. 15 - 20 minutes) the result of the calibration is displayed. Press to store the calculated calibration factors. You might press to print out the factors. By pressing you can repeat the calibration. Press to exit without any changes.

Fig. 6 - 29

Service - Temperature sensor calibration - process finished

Warning: The surface of the calibration accessory is hot. Do not touch the calibration accessory for at least 20 min after finishing the calibration.

6. To avoid entering wrong calibration constants, remove the adhesive label from the sensor arm, if new calibration factors have been stored in the instrument.

6.7.4.2

To Calibrate the T-Probe

1. Put the calibration accessory into the protective casing. Make sure you lead the cable of the calibration accessory to the left side of the protective casing strap.

Fig. 6 - 30

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Putting the calibration accessory in the protective casing

89

6 Software

2. The immersion tube with seal (XF/XQ) can now be put into the calibration accessory. The venting screw has to point to the same direction like the cable of the calibration accessory (left of the protective casing strap).

Fig. 6 - 31

Putting the immersion tube with seal into the calibration accessory

3. Put the protective cap onto the protective casing so that the cable and the venting screw are led through the opening of the cap.

Fig. 6 - 32

Putting the protective cap on the calibration accessory

4. Place the complete vessel assembly together with 3 additional (empty) vessels into Rotor 8S and close the rotor thumb wheels in order to fix the vessels. The calibration accessory has to be placed at position 1.

Fig. 6 - 33

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Inserting the vessel into position 1

90

6 Software

5. Use the glass rod to make sure that the vessel in position 1 is positioned correctly. If there is any resistance when inserting the rod, adjust the vessel and try again. Repeat the procedure until you feel no resistance when inserting the rod.

Fig. 6 - 34

Using the glass rod

Important: Never insert the T-probe unless the vessel is correctly positioned and the rotor is correctly closed, otherwise the glass bulb and the capillary may break!

6. Insert the T-probe very carefully through the hole on the upper plate of the rotor into the vessel at position 1. The torus-shaped part of the T-probe is placed over the sensor module. Adjust the thumb wheels so that the T-probe is attached completely on the rotor upper plate.

Fig. 6 - 35

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Inserting the T-probe

91

6 Software

7. Place the rotor without protection lid into the microwave cavity. Important: Do not close the door of the instrument as this might damage the cable of the calibration accessory.

Fig. 6 - 36


8. Connect the cable of the calibration accessory to the CAL port on the righthand side of the instrument. Tighten the screws of the cable plug to ensure good contact.

Fig. 6 - 37

Connecting the cable of the calibration accessory

9. Press the key to start the calibration. The serial number of the T-probe is read out first. The calibration accessory starts to heat and the temperature values are recorded automatically.

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

Fig. 6 - 38


10. At the end of the heating phase (approx. 15 - 20 minutes) the result of the calibration is displayed on the display. Press to store the calculated calibration factors. You might press to print out the factors. By pressing you can repeat the calibration. Press to exit without any changes.

Fig. 6 - 39


Warning: The surface of the calibration accessory is hot. Do not touch the calibration accessory for at least 20 min after finishing the calibration.

11. To avoid entering wrong calibration constants, remove the adhesive label from the sensor arm, if new calibration factors have been stored in the instrument.

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6.7.5

Temperature Sensor Calibration with the Calibration Unit

For regular calibrations, an optional calibration unit is required to calibrate the p/T sensor (Rotor 48 and Rotor 16) and T-probe (Rotor 8S), respectively. The calibration unit consists of a vessel jacket with an integrated heating block, a Pt-100 temperature sensor for correct measurement of the temperature of the heating block and a metal support. During the calibration the heating block is heated up to two measuring points (40 °C and 180 °C). The difference between the measured temperature values of the heating block and the p/T-sensor is used to calculate two calibration factors.

Important: After carrying out any maintenance o r repair work on the temperatur e sensor, it has to be recalibrated.

Fig. 6 - 40

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Calibration Unit

94

6 Software

Metal support Lock II with two holes Lock I

Calibration insert holder

Front side Back side with counter weight

Cable

Calibration insert

Fig. 6 - 41

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Metal support for the calibration insert and calibration insert

95

6 Software

6.7.5.1

To Calibrate the p/T Sensor

1. Check all parts, which are needed for calibration.

Metal support Calibration insert (T/IR) with cable

p/T sensor Rotor 48 p/T sensor Rotor 16

Fig. 6 - 42

All parts, which are needed for calibration of the p/T sensor for Rotor 48 or Rotor 16

2. Open the metal support (see Fig. 6 - 43 /1). Lift lock I towards the back side of the metal support (see Fig. 6 - 43 /2) to open the interlock. Afterwards raise the pendant (see Fig. 6 - 43 /3) toward the front side until the stop position is reached (see Fig. 6 - 43 /4). The device is automatically fixed in this position.

Back side

Lock I Front side

Fig. 6 - 43

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1

2

3

4

Opening the metal support

96

5 Installation

6. Connect the exhaust hose to the exhaust unit by attaching it to the connecting flange, which is located on the rear side of the instrument. Fix it with the clamp. The foam piece in the exhaust hose reduces the noise and should be positioned in the hose as shown in Fig. 5 - 2.

Fig. 5 - 2

Twisted foam for noise reduction in the exhaust hose

7. Lead the open end of the exhaust hose into an exhaust system or fume hood. Make sure that there is a bypass between the hose of Synthos 3000 and the exhaust system.

Incorrect installation

Fig. 5 - 3

Correct installation

Connection of the exhaust hose to an exhaust system

Warning: Never run the system without the exhaust hose.

8. Check if the plug of the exhaust unit has been inserted properly into the appropriate socket. 9. Connect the mains cable. The socket is located on the rear side of the instrument. 10. Insert the mains cable plug into the wall socket. Synthos 3000 has to be connected to an approved standard wall socket with a ground conductor.

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6 Software

Fig. 6 - 45

Placing the p/T sensor into the calibration insert

5. Place the assembled calibration unit carefully (hold the sensor arm with one hand) into the microwave cavity to avoid scratches to the coating. Take care that the metal support fits as accurate as possible on the turntable. Then connect the cable of the calibration unit to the CAL-port on the right-hand side of the instrument. Tighten the screws of the cable plug to ensure good contact. Important: Do not close the instrument door as this might damage the cable of the calibration insert.

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Fig. 6 - 46

Inserting the assembled calibration unit

6. Select the service menu in the main menu by pressing. 7. Use the arrow keys < F4> and < F5> to select the temperature sensor calibration menu. Confirm by pressing .

Fig. 6 - 47

Temperature sensor calibration - step 1

8. Press the key to start the calibration. The serial number of the temperature sensor is read out first. The calibration insert starts to heat and the temperature values are recorded automatically.

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

Fig. 6 - 48

Temperature sensor calibration - step 5

9. At the end of the heating phase (approx. 15 - 20 minutes) the result of the calibration is shown on the display. Press to store the calculated calibration factors. You might press to print out the factors. By pressing you can repeat the calibration. Press to exit without any changes.

Fig. 6 - 49

Service - Temperature sensor calibration - process finished

Warning: Hot surface! The surface of the calibration insert is hot.

Do not touch the calibration insert for at least 20 min after finishing the calibration. 10. To avoid entering wrong calibration constants, remove the adhesive label from the sensor arm, if new calibration factors have been stored in the instrument. 11. After complete cooling, clean the calibration insert with a damp cloth, if necessary. Let the calibration insert dry completely before next use.

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6.7.5.2

To Calibrate the T-Probe

1. Check all parts, which are needed for calibration.

Rotor 8 (without protection lid) Centering jacket Protective cap Spacer

T-probe Glass rod Calibration insert (T/IR) with cable Immersion tube with seal Fig. 6 - 50

All parts, which are needed for calibration

Protective cap Immersion tube with seal Spacer Cable insert

of

the

calibration

Calibration insert

Centering jacket

Fig. 6 - 51

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Assembled accessory for calibration of the T-probe

101

5 Installation

Fig. 5 - 5

Service - Power calibration

4. Fill 1000 g of tap water (approx. 20 °C) into a beaker (diameter approx. 180 mm). 5. Check if the amount of water in the beaker corresponds to the value shown on the LCD. Possible deviations can be corrected by pressing <+ F2> or . Press .

Fig. 5 - 6

Power calibration - Entering mass of water

6. Select the target microwave power for the calibration. The recommended power is 800 W. Changes can be entered via <+ F2> or <- F3>. Press .

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6 Software

2. Put the calibration insert into the centering jacket. Make sure to lead the cable of the calibration insert through the slot of the casing.

Fig. 6 - 52

Putting the calibration insert into the centering jacket

3. Add the spacer directly on the top of the calibration insert with the two pits on the bottom side. The two screws of the calibration unit have to fit into the two pits.

Fig. 6 - 53

Adding the spacer

4. The immersion tube with seal (XF / XQ) can now be put into the calibration insert. The venting screw has to point to the same direction as the cable of the calibration insert.

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Fig. 6 - 54

Putting the immersion tube with seal into the calibration insert

5. Put the protective cap onto the centering jacket.

Fig. 6 - 55

Putting the protective cap on the centering jacket

6. Place the complete vessel assembly together with 3 additional (empty) vessels into Rotor 8S and close the rotor thumb wheels in order to fix the vessels. The calibration insert has to be placed at position 1.

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Fig. 6 - 56

Inserting the assembled calibration vessel into position 1

7. Use the glass rod to make sure that the vessel (in position 1) is positioned correctly. If there is any resistance when inserting the rod, adjust the vessel and try again. Repeat the procedure until you feel no resistance when inserting the rod

Fig. 6 - 57

Proper positioning by using the glass rod

8. Afterwards close the rotor thumb wheels completely (no movement of the vessels).

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6 Software

6.1

General Information

Synthos 3000 is a software-controlled instrument. Entry of program settings or selection of various instrument parameters are easily done via softkeys on the keypad. Information is provided via the graphic display. All operating elements are integrated in the front panel of Synthos 3000. An external keyboard can be connected to facilitate entry of alphanumerical data. A hierarchical menu structure ensures convenient use of the software and easy instrument operation. The software starts automatically after switching on the instrument. Hint: Periodically check the Anton Paar website (www.anton-paar.com) for software updates or contact our local distribu tor. Install the updated software version according to chapter 6.7.1, "Software Update".

The most impo rtant software features are:

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•

Fast and logical guidance through menu commands

•

Multilingual user interface (v2.0 or higher)

•

Display of all relevant reaction parameters as numeric data and graphs: -

Programmed and actually applied microwave power

-

Individual IR temperatures of reaction vessels

-

Internal temperature of the reference vessel

-

Pressure measurement either inside the reference vessel (Rotor 16 and Rotor 48) or simultaneously in all vessels (Rotor 8)

•

Pressure rate monitoring

•

Automatic reduction of the microwave power if preset limits are reached (pressure, temperature, pressure increase rate)

•

Method library which can be extended as required

•

Automatic control of the exhaust unit (safety cooling)

•

Documentation of process data via external PC or an optional printer

•

Software-assisted calibration of microwave power and optionally available sensors

•

Service and maintenance programs

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6 Software

The keypad consists of the follow ing keys:

•

5 soft keys (F1 - F5) Depending on the menu command, these keys have different functions. The currently active function is shown on the display next to the key.

•

ESC key The key is used to terminate a process and/or move back one step in the menu hierarchy.

•

Start button The green button is used to start a selected method.

•

Stop button The red button is used to interrupt or stop a microwave program.

Softkeys

Current software version Fig. 6 - 1

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Keypad with signal lamp

Assigned functions for softkeys

Start/Stop keys

Operating elements of the Synthos 3000 keypad

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6.2

Basic Software Structure

START

Fig. 6 - 2

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Basic software structure

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6.3

The Main Menu

The main menu appears automatically after switching on the instrument. The installed software version is shown in the lower left corner of the gra phic display.

Fig. 6 - 3

Main menu

The following sections of the program or submenus are accessible via the function keys: •

F1 Library Allows you to select and modify methods or to create new methods. New or modified methods can be saved for future use. Comments can be added to the methods.

•

F2 Review

For viewing and/or printing the stored process data as tables and diagrams (power vs. time, temperature vs. time and pressure vs. time). The available diagrams depend on the sensors used. The stored data can also be sent to an external PC. •

F3 Setup This key accesses a submenu containing different instrument settings.

•

F4 Service This key accesses a submenu containing maintenance and service programs.

•

F5 Info Shows telephone number, fax number and contact e-mail address of Anton Paar GmbH as well as the serial number of the instrument and the

usage information (v2.0 or higher).

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6.4

Library Menu

Starting from the main menu, press to reach the library menu.

Fig. 6 - 4

Library menu

The library menu is used to load stored methods and to create or edit methods using the method editor.

The library menu consists of three areas: • A list of the last four methods used ("Last ") This list is intended for routine operation, i.e. it provides fast retrieval and access to frequently used methods. •

"Make New Sampl e" for creating new methods

•

A method library in alphabetical order ("Library ") This list shows only methods stored for the activated rotors. (Refer to chapter 6.6.5, "Rotors".) To select a method use the arrow keys < F4> or < F5> and < F2> or < F3> and confirm your choice by pressing the key.

To jump directly between these areas, use the arrow keys < F2> or <

F3>.

For various sample materials there may exist several methods using different rotor types. Make sure to select the appropriate method for the rotor used. After selecting a method, the sample menu will be opened.

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6.4.1

Fig. 6 - 5

Sample Menu

Sample menu

The program allows you to select the following functions: •

Start

Starts the selected method displayed in the sample menu. •

Edit Edits the selected method displayed in the sample menu.

•

Notes This option is used to enter a comment or additional information. A flashing notes field indicates information stored for this method.

•

Spl Doc (Sample Documentation) Use this option to enter additional information for each individual reaction vessel. This information is visible during the run and stored in the run-data

only, BUT NOT in the method.

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6.4.1.1

Start

Biginelli

Fig. 6 - 6

Sample menu - Start

By pressing a startup routine is activated, which checks presence and type of rotor in the microwave cavity and verifies whether the rotor has been closed with the protection lid or not. If optional sensors have been installed (e.g. a p/T sensor) and properly configured in the instrument setup, the function of these sensors will also be checked. If an error is detected during the testing procedure, an error message is shown and the method start will be interrupted. If no errors have been detected, the method can be started by pressing the green button.

6.4.1.2

Edit

Depending on the installed rotors and accessories (sensor etc.), the actual sample menu might look different.

Fig. 6 - 7

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Sample menu - Edit

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•

Press <+ F2> and <– F3> to create or change information or parameters for a method. You can use them to enter characters, select options and increase / decrease numerical values.

•

The arrow keys < F4> and < F5> are used to jump between the entry fields.

•

Press to exit the editing dialogue and select one of the following options from the pop-up window: -

-

-

Save:

Press to save your changes by overwriting the (existing) version. This function can be deactivated by locking the method in the library maintenance tool (refer to chapter 6.7.15, "Library Maintenance Tool"). New: Press to store as a new method, the existing one remains unchanged. Discard: Press to cancel your changes. Delete: Press if you wish to delete the method. This function can be deactivated by locking the method in the library maintenance tool (refer to chapter 6.7.15, "Library Maintenance Tool").

Explanation of the entry fields:

•

Sample This field is used to enter a sample name consisting of max. 23 characters

but only 18 will be shown in the library. •

Rotor This field is used to select the rotor type you are going to work with. Deactivated rotors are not displayed and therefore not selectable.

Hint: After selecting the appropriate rotor type, the pressure and temperature limits will be changed automatically.

Important: The HEAT rotor type enables an operating mode that is exclusively for testing purposes (e.g. for service). Misuse of these instructions may result in damage to the Synthos 3000.

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•

Vessels This field is used to enter the number of vessels applied in the rotor. Please follow the recommended loading patterns according to the respective rotor type. Never use less than 4 vessels!

•

Weight

This field is used to enter the weight of your sample material. •

P-Program / T-Program Depending on the type of rotors and sensors, this field can be used to select

a power or temperature program: -

-

P-Program: When using a P-program (power program), the instrument follows a defined power profile and only deviates from this profile when limits such as pressure, pressure increase rate or temperature are exceeded. T-Program: When using a T-program (temperature program), the instrument follows a defined temperature profile and only deviates from this profile when limits such as pressure, pressure increase rate or temperature are exceeded.

Hint: It is highly recommended always to use an immersing temperature sensor,

even when a power program is performed.

•

Ph This field indicates the "Phase“ or step of the power / temperature profile.

•

Power / Temp Power / temperature setpoint at the end of the ramp time.

•

Ramp Time period in which the previously defined power / temperature setpoint has to be reached. Possible range 00:00 to 99:59 [minutes: seconds].

•

Hold Time period wherein the defined power / temperature setpoint has to be held. Possible range: 00:00 to 99:59 [minutes: seconds]. Fan This field is used for setting the intensity of the exhaust unit: - Level 0: minimum intensity (special applications) - Level 1: low intensity (used during heating) - Level 2: medium intensity (for cooling) - Level 3: highest intensity (for cooling)

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•

p-rate The limit of the pressure increase rate is entered in this field. The possible range is between 0.1 - 3.0 bar/s. If the pressure rate exceeds the predefined limit, the microwave generation will be interrupted for a short period of time.

•

IR This field is used to enter the IR temperature limit.

•

p

This field is used to enter the pressure limit for power controlled runs. •

P This field is used to enter the power limit for temperature controlled runs.

•

Drive This field is used to chose the rotor drive mode. Rot.: Constant rotation Osc: Oscillation

•

Stirrer

This field is used for setting the intensity of the stirrer unit in a range of 0 - 3. Off: The magnetic stirrer is switched off. 1, 2 or 3: The magnetic stirrer rotates at varying speeds.

6.4.1.3

Notes

You can enter additional information or notes related to the method in the Notes Editor. The following functions are available:

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•

Start F1 This function is used to start the method directly without going back to the primary menu.

•

Edit F2 This function is used to change existing information or to enter new ones with the alphanumeric keyboard. Leave the Edit mode by pressing the .

•

Sample F3 The key will bring you back to the Sample menu.

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6.4.1.4

Spl Doc (Sample Documentation)

The sample documentation editor can be used to enter additional information with the alphanumeric keyboard. The following functions are available:

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•

Start F1 This function is used to start the method directly without going back to the primary menu.

•

Sample F4 The key brings you back to the sample menu.

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6.5

Review

Starting from the main menu, press to reach the review menu. Run data such as temperature and pressure values are stored automatically during each process. Depending on the number of stored methods, the data of the last 4-8 hours of operation will be available under the review menu option.

Fig. 6 - 8

Review menu

The list is sorted by date / time and offers the following options: •

Enter F1 Press to view the data of the run on the display. Depending on

the type of sensors used, you can select different displays. •

Send Press to send the data of the selected run to an external PC

connected to Synthos 3000 via the serial interface. •

Print Press to print the selected data on a connected printer.

Use the arrow keys <

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F4>, <

F5> to select a stored run.

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6.5.1 6.5.1.1

Review - Displayed Diagrams Rev iew - Nu mer ic

This screen provides an overview (text based) of all maximum values reached during a run.

Max. applied power

Max. pressure

Max. inner temperature or max. applied power

Sample/ Method       

Program duration Fig. 6 - 9

Max. IR temperatures assigned to each vessel

Review - Numeric

Explanation of the data:

•

Power

The max. microwave power [W] which was applied during the run. The applied power may deviate from the maximum power set point defined in the method e.g. if the temperature or pressure limit was reached or the permitted pressure rate was exceeded. •

Temp Maximum inner temperature which was reached in the reference vessel.

•

Pres Maximum pressure which was reached during the reaction.

•

IR

Maximum IR temperatures of reaction vessels and empty positions, respectively.

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IR Lim Temperature limit defined in the method for the IR temperature.

•

T Lim Temperature limit defined in the method for the internal temperature in the reference vessel.

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•

p Lim Pressure limit defined in the method.

•

p Rate Limit of pressure increase rate defined in the method. Hint: Pressure and temperature values will only be available if the reaction was carried out with activated and installed sensors.

6.5.1.2

Rev iew - P-Gr ap h

The review P-graph displays the power and pressure vs. the reaction time.

Programmed power profile Pressure curve

Actually applied microwave power Fig. 6 - 10

Time and reason of the first power reductio n

Review - P-graph

The diagram contains the following information: •

Programmed power profi le If a power program was used the programmed set point is displayed as a dotted line.

•

Ac tu all y ap pl ied mi cr ow ave p ow er The black filled area shows the actually applied microwave power which may deviate significantly from the programmed power profile if pressure, temperature or pressure rate limits are reached.

•

Pressure This curve indicates the pressure course during the reaction.

•

P-reduction time For explanation of the herein stated "control parameters" refer to chapter

11.2.5, "Power Reduction by the Instrument".

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6.5.1.3

Rev ie iew - TT-Gr ap ap h

The review T-graph displays the internal temperature and pressure vs. the reaction time.

(Internal) Temperature

Fig. Fig. 6 - 11

Pressure

Revi Review ew - T-g T-gra raph ph


(Internal) (Internal) t emperature Shows the temperature course in the reference vessel.

•

Pressure

Shows the pressure course during the run.

6.5.1.4

Revie view - IR-Graph raph

The review IR-graph displays the individual IR temperatures and the reaction pressure vs. the reaction time.

IR Temperatures IR Temperature of the empty positions Fig. 6 - 12

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Pressure

Review - IR-graph

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IR temperature Shows the IR temperature curves during a reaction. These data mainly provide information about uniformity of heating. Hint: IR values may differ if varying mixtures are applied in the individual vessels.

•

Pressure Shows the pressure course during the run.

6.5.1. .1.5

Review view - Sample Sample Docume ocument nta ation

This menu item allows the entry of additional sample information. Changes can be entered as necessary. The printout includes date and time of changes, if the changes were done after the run has been completed.

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6.6

Setting tting Up the the Instru nstrume ment nt

Starting from the main menu, press to reach the setup menu. The setup menu is used to change instrument settings. Use the arrow keys < F4> and < F5> to select the desired options from the setup menu. Confirm by pressing .

Fig. Fig. 6 - 13

Setu Setup p - menu menu

The following o ption s are available available in the setup menu:

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Configuration Use this option to set the language (v2.0 or higher), date, time and "device name" and if necessary, make the appropriate layout settings for an external keyboard.

•

Printer Setup This option is used to set the printer type, printer interface and character settings.

•

Serial Serial Port Setup This option is used to set the text compression and transfer delay for data transmission.

•

Safety Safety Cooli ng Set parameters for safety cooling like cooling intensity, cooling time or temperature limits.

•

Rotors Activate / deactivate the appropriate rotor types.

•

Sensors Activate / deactivate the appropriate sensor types.

•

Ac ces so ri es Activate / deactivate accessories.

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6.6.1

Co n f ig ig u r at i o n

Use the arrow keys < F4> and < Confirm by pressing .

Fig. Fig. 6 - 14

F5> to select the configuration menu.

Setu Setup p - Con Confi figu gura rati tion on

Using the keys <+ F2> and <– F3> you may create or change any data or parameters in the entry or option fields, i.e. you may select letters or change between different options. The arrow keys < F4> and < F5> are used to move to the next or return to the previous entry field. Press to store your entries / modifications and revert to the setup menu. Press to exit without saving. The setup configuration section consists of five entry / option fields:

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•

Language Multilingual user interface (v2.0 or higher).

•

Ext. Keyboard Select between the German or English keyboard layout.

•

Device Name Enter an instrument name consisting of max. 12 characters. This name will be stored in the run data and will be printed out.

•

Date Set the current date ("YYYY-MM-DD"). ("YYYY-MM-DD").

•

Time Set the internal clock.

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6.6.2

Pr in in t er Se Set up up

Use the arrow keys < F4> and < F5> to select the printer setup menu. Confirm by pressing .

Fig. Fig. 6 - 15

Setu Setup p - Pri Print nter er setu setup p

The setup printer menu is used to select the connected printer. It consists of four option fields. •

Printer Type The system distinguishes between the following printer types:

-

-

-

-

-

-

•

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Plain Text This setting is for printer models with an internal "character set", i.e. printers that are capable of printing ASCII sequences. This setting can only be used to print text - you will not be able to print any graphs using this setting. Epson 9 Pin This setting is for Epson 9-pin printers or Epson-compatible printers. Used

printer protocol: ESC/P Standard; printing text and graphics. Epson 24 Pin This setting is for Epson 24-pin printers or Epson-compatible printers. Used printer protocol: ESC/P Standard; printing text and graphics. PostScript This requires a PostScript printer (like special laser printers): e.g. HP Laserjet 4 M-plus or a newer model, such as HP 4050n. Used printer protocol: PostScript Language Level 3; printing text and graphics. HP DeskJet This setting is for HP DeskJet printers or HP DeskJet-compatible printers. Used printer protocol: PCL 5; printing text and graphics. HP LaserJet This setting is for HP LaserJet printers or HP LaserJet- compatible printers. Used printer protocol: PCL 5; printing text and graphics.

Printer Port Select Centronics if a printer is connected to the parallel port. Select Serial for sending data via the serial port (RS232) to a connected PC.

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•

Decimal Separator Use this option to select between a period (1.123) or comma (4,567) as decimal separator.

•

Character Set Use this option to select between the ASCII MS-DOS M S-DOS CP437 and ISO 88591 Latin 1 character set, if some characters are not printed correctly.

The <+ F2> and <– F3> keys are used to select the different options. The arrow keys < F4> and < F5> are used to move between the entry fields. Press to save your changes and revert to the Setup menu. Press to discard your entries.

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6.6.3

Ser ia ial Po rt rt Set up up

The serial port setup menu is used to set the parameter for data transfer. Use the arrow keys < F4> and < F5> to select the serial port setup menu. Confirm by pressing .

Fig. Fig. 6 - 16

Setup Setup - Seri Serial al port port setu setup p

The following parameters are available in the serial port setup menu: •

Tex t Co mp mp re res si si on on Text compression reduces the amount of data for faster transfer rates. Data can be imported into a MS Excel irrespective of the used compression mode.

-

-

•

None: No compression, slowest data transfer. Best format for processing with a

text editor. Medium: Character spaces are removed, transfer is accelerated. High: Data duplications are removed, transfer needs only a quarter of the time without compression.

Transf er Delay Depending on the CPU-type and operation system, data transfer without

delay might be too fast for the computer. Increase the transfer delay if you experience problems with the data transfer. -

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For data data transfer transfer to external external PCs PCs via a terminal terminal program program a delay delay is usually usually not necessary n ecessary.. For data data transfer transfer with AP-Sof AP-Softprint tprint we recommen recommend d a transfer transfer delay of at least 30 ms. (Possible transfer delays: None, 10, 20, 30, 50, 100, 250 and 500 ms;)

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6.6.4

Saf et y Co ol ing

The safety cooling menu can be used to adjust the intensity of cooling fan level, cooling time, temperature limit and IR limit. Use the arrow keys < F4> and < F5> to select the safety cooling menu. Confirm by pressing .

Fig. 6 - 17

Setup - Safety cooling

The safety cooling system is activated: • • • •

After terminating the experiment. An unexpected reset of the instrument, e.g. after a power failure. If no cooling step has been programmed in the method.

Cooling Fan Level Press the <+ F2> or <– F3> key to select between cooling fan level 2 and 3.

-

-

Cooling Fan Level 3 Highest intensity (190 m3/h). Benefit: Short cooling time. The minimum cooling time is 30 minutes. Cooling Fan Level 2 Medium intensity. Benefit: Lower noise level. The minimum cooling time is 60 minutes.

Hint: After an overpressure release inside the cavity (e.g. safety disk or vessel breakage), the safety cooling will always run on fan level 3.

•

Temperature Li mits Depending on the used sensors, you can choose the temperature values, which have to be reached during the cooling process. Default settings for synthesis applications are 60 °C for internal temperature and 50 °C for IR

temperature, both limits can be reduced down to 40 °C. Please note that reducing these values will result in increased cooling times.

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6.6.5

Rotors

Rotor types have to be activated before they can be used! Use the arrow keys < F4> and < F5> to select the rotors menu. Confirm by pressing .

Fig. 6 - 18

Setup - Rotors step 1

Move the black cursor to the desired rotor type using the arrow keys< F4> and < F5>. Activate or deactivate the selected rotor type by pressing <+ F2> or <– F3>. Press to confirm the changes. Press to exit without saving the changes. The current status is displayed by a symbol, which is shown to the left of the selected rotor type: -

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Empty rectangle : Rotor is deactivated. Filled rectangle : Rotor is activated.

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6.6.6

Sensors

Sensors have to be activated before they can be used! Use the arrow keys < F4> and < F5> to select the sensors menu. Confirm by pressing .

Fig. 6 - 19

Setup - Sensors

Move the black cursor to the desired sensor using the arrow keys < F4> and < F5>. Activate or deactivate the selected sensor by pressing <+ F2> or <– F3>. Press to confirm the changes. Press to exit without saving the changes. The current status is displayed by a symbol, which is shown to the left of the selected sensor: -

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Empty rectangle : Sensor is d eactivated. Filled rectangle : Sensor is activated.

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6.6.7

Accessories

Accessories have to be activated before they can be used! Use the arrow keys < F4> and < F5> to select the sensors menu. Confirm by pressing .

Fig. 6 - 20

Setup - Accessories

Move the black cursor to the desired accessory using the arrow keys< F4> and < F5>. Activate or deactivate the selected accessory by pressing <+ F2> or <– F3>. Press to confirm the changes. Press to exit without saving the changes. The current status is displayed by a symbol, which is shown to the left of the selected accessory: -

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Empty rectangle : Ac ces so ry is deac ti vat ed . Filled rectangle : Ac ces so ry is act iv ated .

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6.7

Service

The service section of the software includes calibration and maintenance programs. Use the arrow keys < F4> and < F5> to select the service menu. Confirm by pressing .

Fig. 6 - 21

Service menu

The following options are available in the service menu: •

Software Update For updating the software (requires an external PC)

•

Power Calibratio n For adjusting the microwave power output

•

Power Check

For checking the microwave power output •

Temp. Sensor Calibration For calibration of temperature sen sor (p/T sensor or T-probe)

•

Temp. Sensor Check For checking the accuracy of temperature sensor (p/T sensor or T-probe)

•

Tem p. Sen so r Set ti ng s For entering the calibration factors of temperature sensor (p/T sensor or Tprobe)

•

IR Sensor Calibratio n For adjusting the IR sensor

•

IR Senso r Check

For checking the IR sensor •

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Solvent Sensor Setting s For entering the calibration factors of the solvent sensor

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•

Exhaust Unit Installation For changing the exhaust unit settings

•

Libr ary Maintenance Tool For managing the methods of the method library.

•

Ad van ced Serv ic e Rou ti nes This program section includes special service programs. Access to this option is password-protected and restricted to authorized service engineers.

6.7.1

Soft war e Upd at e

Hint: We recommend to check regularly for new software versions (http:// www.anton-paar.com) and to install if appropriate.

The following equipment is required:

-

-

External PC with a free serial interface, Windows 98 or higher with NET 2.0 (v2.00 or higher) (Alternatively: External PC with USB port, serial-to-USB converter cable) Serial link (0-Modem) cable, this cable is also available from Anton Paar GmbH or its sales representatives Flash update program for Synthos 3000 (available from Anton Paar GmbH free of charge) Synthos 3000 software installation file(s) (available from Anton Paar GmbH free of charge)

Press to enter the software update menu. Connect the host computer´s serial port and run the program Flash Update to activate the bootloader. Follow the instructions given therein to pr oceed with the update.

6.7.2

Po wer Cal ib rat io n

The purpose of this calibration procedure is to adjust the microwave power parameters to ensure accurate values for the applied power output. The calibration is based on the knowledge of the specific heat capacity of water. By heating up a certain amount of water with microwave energy, the apparent power can be calculated from the water volume, the temperature of the water before and after heating. The power calibration consists of the following steps which are carried out automatically by the software:

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-

Determining the apparent power output of the microwave generators Calculating a power factor

Use the arrow keys < F4> and < F5> to select the power calibration menu. Confirm by pressing .

6.7.2.1

To Perform a Power Calibration

To perform a power calibration, refer to chapter 5.5, "Microwave Power Calibration".

6.7.3

Power Check

The power check function is used to verify the microwave power calibration. The procedure is the same as described for the power calibration, but at a target power of 1400 W.





Fig. 6 - 22

Service - Power check finished

Hint: If the apparent microwave power deviates from the nominal value by more than 10% a microwave power calibration should be performed.

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6.7.4

Temperature Sensor Calibration with the Calibration Ac ces so ry

For regular calibrations, an optional calibration accessory is required to calibrate the p/T sensor (Rotor 16) and the T-probe (Rotor 8S). Calibration should be done once a year, although it is recommended to calibrate the temperature sensor at least twice a year. Hint:

Description only valid for calibration accessory up to version 4. If you are using a calibration unit, please follow the instructions in chapter 6.7.5, "Temperature Sensor Calibration with the Calibration Unit".

Use the arrow keys < F4> and < F5> to select the temperature sensor calibration menu. Confirm by pressing .

Version 4

Fig. 6 - 23 6.7.4.1

Calibration accessory To Calibrate the p/T Sensor

1. Carefully insert the p/T sensor into the calibration accessory and close the screw cap.

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Fig. 6 - 24

Inserting the p/T sensor into the calibration accessory

2. Place the calibration accessory with the temperature sensor into position 1 of your rotor and place the rotor without lid into the microwave cavity.

Fig. 6 - 25

Inserting the calibration accessory

Important: Do not close the instrument door as this will damage the cable of the calibration accessory.

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4.8.2

Fu nc ti on Ver if ic at io n

The function verification is only used for testing the sensor. For the function verification you will need acetone and a 1 or 1.5 L bottle (any material), which can be closed with a screw cap.

4.8.2.1

To Verify the Function

1. Check if the Solvent Sensor Accessory is installed and connected to the instrument. 2. Switch on the instrument and wait until the Solvent Sensor Accessory has reached a minimum temperature of 36 °C. 3. Open the Service - solvent sensor setting dialogue.

Fig. 4 - 20

Service - Solvent sensor settings

4. Check if the calibration constant is entered (available from the calibration certificate or determined by performing the user calibration). 5. The "Value" is proportional to the measured solvent concentration in the exhaust channel. 6. Open the door of Synthos 3000. 7. Remove the turn table and driving star. 8. Press for the test mode. The exhaust unit is set to level 1. 9. Fill acetone into the bottle (0.5 mL acetone per 1L bottle volume). Close the bottle with the screw cap and shake it for at least 30 seconds. 10. Hold the bottle upside down onto the exhaust holes in the cavity and open the screw cap. 11. The signal on the display should reach a minimum value of 1000-1500. If not, contact your local customer service.

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4.8.2.2

To Calibrate the Solvent Sensor Accessory

Important:

Calibration of the Solvent Sensor Accessory has to be done reg ularly.

Warning: Always wear goggles, protective gloves and appropriate protective clothing when handling solvents and observe the relevant national regulations.

For calibration of the Solvent Sensor Accessory it has to be put on a volumetric flask. During the calibration in a volumetric flask the solvent sensor will be tested in a standardized atmosphere to determine the sensitivity of the sensor during use. After applying a certain amount of solvent, the signal of the sensor can be stored as the new calibration factor. Tools required for calibration: -

measuring cylinder (volume: approx. 1L, diameter: > 7 cm) solvent for calibration (acetone, hexane or methanol) solvent syringe (volume: 0.1 - 0.25 mL) adhesive tape

1. Switch off the instrument. 2. Remove the sensor in reverse order to the installation procedure. Refer to chapter 4.8.1.1, "To Install the Solvent Sensor Accessory". 3. Connect the Solvent Sensor Accessory to the AUX port of Synthos 3000.

Cable of the Solvent Sensor Accessory

Fig. 4 - 21

Connecting the Solvent Sensor Accessory to Synthos 3000

4. Switch on the instrument. 5. Use the arrow keys < F4> and < F5> to select the solvent sensor settings menu in the service menu. Confirm by pressing .

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6. Wait until the Solvent Sensor Accessory has reached a minimum temperature of 36 °. 7. Close the measuring cylinder with the Solvent Sensor Accessory.

Fig. 4 - 22

Solvent sensor on a measuring cylinder

8. Use an adhesive tape for sealing. Take care for proper sealing.

Fig. 4 - 23

Sealing with an adhesive tape

9. Depending on your application inject one of the following solvents into the measuring cylinder (through the adhesive tape): • •

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n-Hexane: 32 μL for 50 % lower explosion limit methanol/acetone: 56 μL for 50 % lower explosion limit

43


n-Hexan or Methanol/acetone Fig. 4 - 24

Injecting the solvent

10. Shake the measuring cylinder and read out the highest signal value on the display of the instrument.

Signal value

Fig. 4 - 25

Service - Solvent sensor settings

11. Remove the sensor from the measuring cylinder and vent the flask by purging with an air stream. 12. Repeat these steps 2 times and enter the average value into the instrument as your new "Calib. Constant". 13. A variation of the signal of +/- 200 between the different trials is within the specified operation limits. If the limits excess the variation of +/- 200, contact your local customer service.

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4.9

Technical Description of the Magnetic Stirrer Device

Fig. 4 - 26

Magnetic stirrer device

The magnetic stirrer device is a useful tool for mixing the contents of the closed reaction vessels inside Synthos 3000. Depending on the application, stirring helps to obtain better recoveries or to attenuate spontaneous reactions by avoiding local inhomogeneity inside the vessels. The magnetic stirrer device is installed underneath the cavity and consists of three plates with strong permanent magnets, which drive the magnetic stir bars inside the reaction vessels. Different rotation speeds (200, 400 and 600 rpm) are selected and controlled via the software.

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5 Installation

5 Installation The following chapter explains the requirements and the steps to be performed for a successful installation of Synthos 3000.

5.1 5.1.1

Installation Requirements Ex haus t Sy st em

Important: A reliable exhaust system with sufficient capacity (min. 300 m³/h) must be provided when operating Synthos 3000. Hazardous and noxious gases may build up if an appropriate and working exhaust system is not provided at the place of installation. Synthos 3000 must

not be set in operation in this case. Synthos 3000 must be installed in an operating fume hood and following enquiries have to be fulfilled:

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•

Provide easy access to the instrument, especially to the connection ports on the right hand side.

•

A clean surface or workbench should be available next to the instrument for manipulating the rotors.

•

Provide sufficient clearance (10 cm) between the instruments side panel and rear panel, respectively, and the laboratory walls for satisfactory circulation of the cooling air.

•

The exhaust tube must be routed with a sufficient bending tolerance to prevent it from being squeezed or kinked.

•

The utilized fume hood must be operating and switched on during the experiments to withdraw vapors and gases, especially after venting actions.

•

No reagents or samples should be placed on top or right next to the instrument.

•

The surrounding environment of the instrument must be kept scrupulously clean.

•

Any spills of chemicals, solvents, etc. must be removed IMMEDIATELY using appropriate equipment.

•

The valid Laboratory Safety Regulations must be observed.

Regulations

and

Occupational

Safety

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5 Installation

5.1.2

Electrical Requirements

Warning: Synthos 3000 must be connected ONLY to an approved standard socket with protective conductor! Before plugging in the cable, always make sure that the local mains supply and frequency correspond to the values on the type plate of the instrument.

Synthos 3000 requires a constant supply of electrical current, corresponding to the values listed below. The power supply must meet the local safety regulations.

Mains supply

AC 230 V ± 10 %

Frequency

50 Hz ± 0.3 Hz or 60 Hz ± 0.3 Hz

Line protection (fuse)

at least 16 A (USA and Canada: at least 20 A); tripping characteristics type "C", according to IEC 898

Current supply

at least 16 A (USA and Canada: at least 20 A); tripping characteristics type "C", according to IEC 898

The rating of each Synt hos 3000 instru ment (voltage and fr equency) is print ed on the type plate on the rear side of the instrum ent.

The instrument is delivered with an appropriate mains cable. 50 Hz instruments

2.5 meter, line power cable with CEE plug, IEC 309 250 V, 16/20 A, 2-pole, plus protective earth

60 Hz instruments

2.5 meter, line power cable with NEMA L620R Twistlock plug, 208-240 V, 60 Hz, 20 A, 2-pole, plus protective earth

If your laboratory is equipped with another plug system, you have to provide a suitable and approved connection cable.

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5 Installation

5.2

Installation Steps

For detailed information follow the instructions given on the video manual on CD. 1. Unpack Synthos 3000 and inspect it for possible signs of damage in transit. Important: Keep the packing material for transporting the instrument at a later time (change of location, repair, upgrade etc).

2. Make sure that the door can be closed properly and the sealing surfaces of the door are not damaged.

Warning: Never operate Synthos 3000 if the doo r is damaged! In this case the function of the safety features can no longer be guaranteed and harmful microwave radiation may escape.

3. If the instrument has been transported at low temperatures (e.g. in winter), please allow it to adjust to room temperature before switching it on! 4. Check if the voltage and frequency are in accordance with the ratings on the instrument label. Important:

When lifting Synthos 3000, only hold it by the outer edges of the base. Never lift Synthos 3000 by the instrument door. Never transport Synthos 3000 with a rotor inserted.

5. Check the proper installation of the foam seal between tube and exhaust unit.

Fig. 5 - 1

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Checking the proper installation of the foam seal

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5 Installation

11. Switch on the mains switch of Synthos 3000. The mains switch is located at the front below the instrument door. 12. Adjust the view angle of the LCD after the software has started automatically. The knob is marked "VIEW ANGLE" and located on the upper right-hand side of Synthos 3000. By turning the knob you can adjust the LCD for optimum readability. 13. Rotors and accessories of Synthos 3000 have to be activated and configured via the software before use. For detailed information read chapter "Software" in this reference manual.

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6 Software

3. Attach the calibration insert to the ring on the front side of the metal support (see Fig. 6 - 44 /1). Be aware that the two screws have to be at the side of the lock II (see Fig. 6 - 44 /2). Lift the lock II, hold it and push the calibration insert back to the fixed pendant (see Fig. 6 - 44 /3). Release the lock II, the two screws have to fit into the two holes and then the calibration insert itself is fixed (see Fig. 6 - 44 /4).

Screws

Lock II with two holes

1

3

Fig. 6 - 44

2

4

Attaching the calibration insert to the metal support

4. Put the corresponding p/T sensor into the calibration insert. Be aware that the arm of the p/T sensor rests between the two screws on the upper side of the metal support.

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5 Installation

5.3

5.3.1

Connecting Accessories

Printer

Reaction data can be printed for documentation. All printer models with an installed ASCII character set are suitable for printing text documents (without graphs). If you wish to print text and graphs, e.g. pressure / temperature curves, you may connect any compatible printer. The printer port is located on the right side of the instrument and marked "PRINTER".

5.3.2

Keyboard

An alphanumeric keyboard can be connected to Synthos 3000. This keyboard allows you to edit methods and enter new ones. The appropriate port is marked with "KEYB" and located on the right side of the instrument.

5.3.3

Ex ter nal Co mp ut er

Reaction data can be transferred to an external PC via a serial interface. The port "COM1" is provided on the right side of the instrument. This RS232 interface is an SELV (safety extra-low voltage ) circuit that can only be connected to other SELV or SELV-E circuits. Only use shielded cables with a length of less than 3 m for this connection. A standard terminal program can be used to store the run data as text file on an optionally computer. The free Excel Add-in "AP-Softprint for Synthos 3000" (available at AP-Website) can be used to import the run data directly into a MS-Excel sheet, which simplifies both, data collection and diagram generation. For connection to a PC / notebook without serial interface, a serial-to-USB converter is available.

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5 Installation

5.4

Activating / Deactivating Rotors, Sensors and Ac cessories

Prior to the first reaction with Synthos 3000, proper instru ment settings have to be checked and the appropriate rotor types and accessories have to be activated in the setup menu. Hint: All rotors, sensors and accessories for Synthos 3000 which are added or put into operation must be activated and configured before first use. You can also deactivate rotors, sensors or accessories which are no longer required.

Starting from the main menu, press to reach the setup menu. The setup menu is used to change instrument settings. The arrow keys < F4> and < F5> are used to select the desired options from the setup menu, which are subsequently confirmed with .

Fig. 5 - 4

Setup - menu

Refer to chapter 6.6, "Setting Up the Instrument".

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5 Installation

5.5

Microwave Power Calibration

The purpose of this calibration procedure is to adjust the microwave power parameters to ensure accurate values for the applied power output. Hint: Microwave power must be calibrated before the first reaction and can be repeated at periodical intervals. Calibrate the microwave power at 800 W maximum as described below.

Required material:

• • • •

Immersion thermometer with a resolution of 0.1 °C Balance with a weighing capacity of at least 1000 g water in for example a 1 L volumetric flask. 1 L glass beaker with a diameter of approx. 180 mm Tap water (temperature approx. 20 °C)

The calibration is based on the knowledge of the specific heat capacity of water. By heating up a certain amount of water with microwave energy, the apparent power can be calculated from the water volume, the temperature of the water before and after heating. The power calibration consists of the following steps which are carried out automatically by the software: -

Determining the apparent power output of the microwave generators Calculating a power factor

The list below is a short description of the power calibration procedure: 1. Switch on Synthos 3000. 2. Press to select the service menu. 3. Press < F5> to select the power calibration option. Confirm by pressing .

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5 Installation

Fig. 5 - 7

Power calibration - Selecting the target microwave power

7. Measure the temperature of the water. Use the <+ F2> or <- F3> key to enter the measured temperature value, then press .

Fig. 5 - 8

Power calibration - Entering the temperature of the water

8. Open the door of Synthos 3000 and place the beaker on the turntable. Close the door.

Fig. 5 - 9

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Power calibration - Start heating for calibration

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                                                        

                        

Reference Manual Synth yn thos os 3000 Microwave Synthesis

5 Installation

Fig. 5 - 12

Power calibration - Entering the water temperature

The microwave power factor will now be calculated and displayed.

Fig. 5 - 13

Power calibration - Saving the power factor

11. Press to store the new power factor. Press to repeat the power calibration once again. Press if you want to print out the calculation for documentation purposes. If the calculated power ratio is out of range (v1.52 or lower: 0.8 - 1.2; v2.0 or higher: 0.7 - 1.3) saving is not possible. In this case enter either 0.8 (if the power ratio was below 0.8) or 1.2 (if the power ratio was above 1.2), press and repeat the calibration procedure with the new settings (). Press to exit without any changes.

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Synthos 3000 Reference Manual

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