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Summary of Contents for CEM liberty
- Page 1 Operation Manual 600178 Rev. 5...
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Page 3: Table Of Contents
Waste Disposal System Requirements Bench and/or Fume Hood Space Environmental Conditions Inert Gas Source Electrical Requirements Section 2: Operation of the Liberty Introduction to the Liberty Components and Parts Reaction Vessel Components Introduction to PepDriver PepDriver Main Screen Control Buttons... - Page 4 Loading a Method Loading Multiple Methods Preparing Reagents Standard Concentrations Preparing Activator Solution Preparing Activator Base Solution Preparing Amino Acids Preparing Deprotection Solution Preparing Capping Solution Preparing Cleavage Solution ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009...
- Page 5 Creating a Run History Report Sample Run History Report Section 3: Quick Setup Guide Peptide Setup Create and Load the Method Prepare Reagents Ensure the Liberty is Ready to Run Section 4: Mainteance of the Liberty Routine Maintenance Daily Maintenance Weekly Maintenance Biweekly Maintenance...
- Page 6 Low Pressure Adjustment Leak Check Test Rotary Valves Internal, Nitrogen, and Liquid Delivery Tests Setting Up the Liberty for a Delivery Test Performing a Delivery Test Test Sensors Reagent, Amino Acid, and External Amino Acid Addition Leak Check Reaction Vessel...
- Page 7 Bottle Tubing Assemblies Bottle Caps Dip Tubes O-Rings Valves and Valve Wiring Liquid Sensors Waste Container Accessories and Tools Computer Accessories Circuit Boards Regulators Documentation Section 8: Index Liberty ™ Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009...
- Page 8 ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009...
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Page 9: Section 1: Introduction
Section 1: Introduction Introduction About This Manual This manual (PN 600178) describes the operation and maintenance of the Liberty™ Automated Microwave Peptide Synthesizer. The manual is intended for use by both novice and experienced users. This introductory section contains a list of common abbreviations and units used throughout the manual, as well as important information for the safe operation of the unit. -
Page 10: Common Abbreviations And Units
N-((dimethylamino)-1H-1,2,3-triazolo-4,5-bi- pyridin-1-yl-methylene) N-methylmethan- aminium hexafluorophosphate N-oxide HBTU 2-(1 H-benzotriazol-1-yl)-1,1,3,3- tetramethyl-uronium hexafluorophosphate HCTU O-(6-chlorobenzotriazol-1-yl)-N,N,N’,N’- tetramethyluronium hexafluorophosphate hydrofluoric acid HOAt 1-hydroxy-7-azabenzotriazole HOBt 1-hydroxybenzotriazole Hertz inner diameter liter length meter ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... - Page 11 PyAOP (7-Azabenzotriazol-1-yloxy) tripyrrolidinophosphonium hexafluorophosphate PyBOP (Benzotriazol-1-yloxy) tripyrrolidinophosphonium hexafluorophosphate reaction vessel seconds TBTU O-(Benzotriazol-1-yl)-N,N,N′,N′- tetramethyluronium tetrafluoroborate trifluoroacetic acid triisopropylsilane trityl volts of alternating current Watts width ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009...
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Page 12: How To Obtain Support
From the website requests for phone or email support can also be submitted. CEM is proud to provide technical support for the Liberty from a team of specially trained Service Technicians. For technical support in the US and Canada, call (800) 726-5551 or (704) 821-7015 and ask for “Liberty Service”. -
Page 13: Contact Cem
3100 Smith Farm Rd Matthews, NC 28104 Email (Applications Support): peptides@cem.com Email (Technical Support): service@cem.com CEM International Subsidiaries France: CEM mWave S.A.S. Phone: (33-1) 69 35 57 80 Fax: (33-1) 60 19 64 91 Address: Immeuble Ariane Domaine Technologique de Saclay 4, rue René... -
Page 14: Cem Distributors
Buckingham Great Britain Email: info.uk@cem.com CEM Distributors For a complete list of distributors of CEM products, including contact information, go to the CEM website (http://www.cem.com), select Contact Us, and then select Distributors. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 15: Safety Information
A WARNING is intended to provide emphasize dangerous or hazardous conditions which may result in personal injury to the user and damage or destruction of the instrument. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 16: Safety Information
System Requirements Bench and/or Fume Hood Space The Liberty should be positioned on the bench such that access to the electrical outlets for the system is not restricted. The Liberty requires the following space for system components: Liberty Instrument (Discover Module and Liberty Module): 30”... -
Page 17: Environmental Conditions
Relative Humidity Range: 0 – 85% Inert Gas Source The Liberty requires an inert gas source (either high purity grade nitrogen or argon) capable of supplying 25 psi (20 L/min flow) within ten feet (10’)/three meters (3 m) of the right side of the instrument. -
Page 18: Section 2: Operation Of The Liberty
Liberty Introduction to the Liberty The Liberty Automated Microwave Peptide Synthesizer is the first and only automated microwave peptide synthesizer. Built on CEM’s flexible Discover microwave platform, the Liberty is capable of synthesizing up to twelve peptides in sequence on scales ranging from 0.05 to 5 mmol faster and more efficiently than conventional synthesizers thanks to the system’s patented circular... - Page 19 External Amino Acid 3-Port Amino Acid Manifolds Manifold Manifold Resin Manifold Product Manifold Waste Lines Filters Solvent Deprotection Power Lines and Capping Switches ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009...
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Page 20: Components And Parts
Components and Parts • The Liberty handles all of the fluid transfer into and out of Liberty Module: the reaction vessel. In addition, the Liberty manages communications with the computer controller and the Discover during peptide synthesis. • Discover Microwave Reactor: The Discover microwave reactor holds the reaction vessel and generates the microwave energy used to irradiate the sample. -
Page 21: Reaction Vessel Components
0.025 mmol. Reaction Vessel Components Fiber Optic Filter Probe Drain Line Spray Head Quick Disconnect Thermowell Resin Tube Glass Frit ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 22: Introduction To Pepdriver
Introduction to PepDriver The operation of the Liberty is controlled through the PepDriver software package. The Liberty includes an external computer controller (either a laptop or desktop Windows PC) for running PepDriver. This computer is connected to the Liberty and the Discover through an ethernet connection. -
Page 23: Pepdriver Main Screen
Menu Buttons Control Methods Buttons Sequences Estimated Time Start Cycles Remaining Pause Setup Stop Maintenance Calculator Peptide Synthesis Status Resin Positions Tabs Current Method Detail System Status Line ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 24: Control Buttons
Resin Positions: The twelve positions on the screen correspond to the twelve positions on the resin manifold of the Liberty. The resin should be loaded in the same position on the manifold as the method has been loaded into in PepDriver. -
Page 25: Tabs
• Queue: This tab shows all currently loaded Methods. From this tab, the order that each Method is run in can be changed. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 26: Revision 5 • October
Run History: From this tab, detailed logs of each Method that has been run can be accessed. In addition, Method Reports can be generated for each Method that has been run. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 27: Editors
5 °C below the set temperature. The total agitation time can also be selected. • Multi-Step: Multi-Step methods allow for a single microwave method to use multiple power, temperature, or time settings. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 28: Creating A New Microwave Method
High Pressure bubbling is not recommended as this can deposit resin on the top of the reaction vessel. This can lead to poor synthesis quality, product loss, and contamination between syntheses. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 29: Editing An Existing Microwave Method
Open the folder of the appropriate method type, then open the subfolder for the appropriate scale. Click on the microwave method to be modified. Make any changes as needed. Click Save to save the changes to the method. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 30: Cycle Editor
A cycle will only appear in the Method Editor when creating a method of the same scale. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 31: Cycle Types
Step 1 will appear in the cycle window. Operation box and select the operation to be performed. (For a full list Click the of available operations, see Appendix 3: Operations in the Cycle Editor.) ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 32: Editing An Existing Cycle
Open the folder for the appropriate cycle type, then open the subfolder for the appropriate scale if necessary. Click on the cycle to be modified. Make any changes as needed. Click Save to save the changes to the cycle. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 33: Copying And Modifying An Existing Cycle
NOTE When copying a cycle to use with a different scale, verify that the volumes used are appropriate for the new scale before using the cycle. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 34: Sequence Editor
Click the white Sequence box at the bottom of the Sequence Editor. 4.2.2. Type the sequence (N-terminus to C-terminus) using the one letter abbreviations. Click Save to save the sequence. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 35: Modifying A Sequence
Enter the protected and unprotected molecular weights for the amino acid being used. Click OK. The Amino Acid Weight configuration window will close, and the unprotected weight will appear in the MW box next to the button. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 36: Importing A Sequence
If using Excel 2007 or later, the file must be saved as an Excel 97-2003 compatible file (.xls, not .xlsx). The file name should be in English. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... - Page 37 The Import window will be updated to reflect the successful import of the sequences. The imported sequences are now available for use in the Sequence Editor and Method Editor. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009...
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Page 38: Method Editor
Skip Resin Load: This will skip the initial loading of the resin into the reaction vessel. Select this option only if the resin has been placed directly into the reaction vessel. This will also skip the resin swelling step. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... - Page 39 NOTE The substitution value entered here will not affect the operation of the Liberty. It is only needed for the Usage Calculator to calculate how much resin is required for the synthesis. 8. Assign cycles for each residue in the sequence that will not use the default cycle.
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Page 40: Modifying An Existing Method
Click on the method to be modified. The sequence will automatically be selected and loaded. Make any changes to the method as needed. Click Save to save the changes to the method. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 41: Calculators
Load any methods to be run by dragging them to the appropriate resin positions (see p. 46). Click on the Calculator button, and select Usage from the menu. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 42: Reagent Calculator
There are six tabs: Resin, Deprotectors, Bases, Activators, Amino Acids, and Cleavage. NOTE The Reagent Calculator contains a library of common reagents. The Liberty is not limited to only these reagents; however, the Reagent Calculator can only perform calculations using reagents in the library. -
Page 43: Deprotection Calculator
The default concentration is 2 M. DIEA should be prepared using NMP as the solvent because of its miscibility in DMF. Enter the total volume of activator base solution needed. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 44: Activator Calculator
All box. Enter the total volume of amino acid solution. Click Calculate. The calculator will report the required amount of amino acid(s) in grams. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 45: Cleavage Calculator
When all of the percentages are correct, the required amount of each reagent to be added will be displayed in grams (for solids) and mL (for liquids). NOTE CEM recommends using 95% TFA, 2.5% TIS, 2.5% DODT, and 2.5% water as the cleavage cocktail. ™ Liberty Automated Microwave Peptide Synthesizer 600178 •... -
Page 46: Setting Up A Synthesis
To load by dragging: Open the appropriate folder in the Methods tab. Click on the desired method, and drag the method to the appropriate resin position. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 47: Loading Multiple Methods
Preparing Reagents Standard Concentrations The Liberty uses stock solutions of all reagents. The default cycles are designed to deliver enough of each stock solution to give 5 eq of amino acid and activator and 10 eq of activator base for each coupling. The table below details the standard concentrations used on the Liberty. -
Page 48: Preparing Activator Solution
Preparing Amino Acids CEM offers a full line of pre-weighed amino acids in 5 mmol, 10 mmol, and 20 mmol sizes. It is not required to use the pre-weighed amino acids. To use CEM pre-weighed amino acids: Open the bottles, breaking the safety seals. -
Page 49: Preparing Deprotection Solution
Capping is optional, and is not necessary for most routine syntheses. The capping bottle does not need to be in place unless capping is being used in the method(s) being run. CEM recommends using 0.5 M acetic anhydride in DMF with 0.125 M DIEA and 0.015 M HOBt. To... -
Page 50: Preparing Cleavage Solution
WARNING TFA should only be connected to the Cleavage position. The use of TFA on any other position will cause serious damage to the Liberty. 3. Load deprotection and capping (if needed) using the Change Bottle command. (For more information about the Change Bottle command, see p. 65.) 3.1. -
Page 51: Revision 5 • October
Ensure the dip tube has a dip tube filter in place, then screw the cap onto 3.4. the deprotection bottle. 3.5. Click Next to continue with the Change Bottle procedure. The Liberty will automatically pressurize the bottle and ensure the lines are filled and ready to add. 3.6. -
Page 52: Loading Resin Onto The Liberty
Remove the 35 mL (Standard) reaction vessel from the microwave cavity. Carefully remove the temperature probe from the thermowell. Disconnect the four lines from the manifold on the front of the Liberty. Place the 10 mL vessel into the microwave cavity, securing the attenuator. -
Page 53: Running The Liberty
WARNING If the probe is not inserted all the way to the bottom of the vessel the Liberty will not accurately measure the temperature, and significant overheating of the vessel will occur. -
Page 54: Running The Liberty
Verify the 125 mL vessel is connected and then click OK to continue. The Liberty will go through a series of initialization steps to ensure all valves are in the correct positions and that there is sufficient nitrogen pressure. - Page 55 The current step of the method is highlighted in yellow in the Current Method Display. The Liberty will enter a wait state for 15 minutes following resin transfer to allow the resin to swell. The time remaining (in seconds) will be displayed on the System Status Line.
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Page 56: Generating Reports
Right-click on the specific run to be reported and select Display Method Report. The Report Viewer window will open, and the method report will be rendered as a PDF. Click Save As PDF to save the report. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 57: Sample Method Report
Cleaving 35min Transfer Product Cleaved Add Reagent Transfer Product Cleaved Add Reagent Transfer Product Cleaved Clean Reaction Vessel - Unfiltered 10.0 Reaction Vessel Neutralization 10.0 Wash - Top ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 58: Run History Reports
Wash - Cycle 1 of 1 7/17/2009 10:12:06 AM DMF (5.5/5.7) 7/17/2009 10:12:46 AM Add Reagent: Deprotect Deprotect (4.9/0.0) 7/17/2009 10:13:19 AM 7/17/2009 10:14:07 AM Microwave: Deprotection - Power: 35 Watts ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 59: Section 3: Quick Setup Guide
Section 3: Quick Setup Guide Liberty Setup Create and Load the Method 1. Create a new sequence. Open 1.1. Sequence Editor by clicking on the Sequence button at the top. 1.2. Click on the folder where the sequence should be saved, then click the New Sequence button. -
Page 60: Prepare Reagents
Method Tab and dragging it to one of the resin positions at the top of the screen. Each position corresponds to one of the twelve resin positions on the front of the Liberty. The resin position should turn green. Prepare Reagents... -
Page 61: Ensure The Liberty Is Ready To Run
Verify that the fiber optic probe is fully inserted into the thermowell. WARNING If the probe is not inserted all the way to the bottom of the vessel the Liberty will not accurately measure the temperature, and significant overheating of the vessel will occur. - Page 62 Method Editor. 8.4. Load the corrected method as described in step 3. If the method is correct and all reagents are attached to the Liberty, press the Start button at the top of the screen to begin the synthesis. NOTE If the Method is for 0.5 mmol scale or larger, a warning to verify that the 125...
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Page 63: Section 4: Mainteance Of The Liberty
Liberty Routine Maintenance A routine maintenance protocol is vital for the long-term operation of the Liberty. Further details about the maintenance procedures can be found in the Liberty Maintenance Procedures Manual (PN 600119). The Liberty Maintenance Procedures Manual also contains twelve months of maintenance logs for recording and maintaining maintenance records. -
Page 64: Semiannual Maintenance
Liberty is heating properly. The temperature for a coupling should reach 75 °C within 70 seconds. If the Liberty is not reaching temperature in time, increase the power setting in the Microwave Editor (see Editing an Existing Microwave Method, p. -
Page 65: Maintenance Screen
Depressurize: Clicking this button will vent any pressure from the reagent selected from the pull-down menu. • Clean All Manifolds: Clicking this button will begin a cleaning procedure for ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... - Page 66 For more information about using the Backflush command, see Performing a Backflush, p. 65. • Backpurge: Clicking this button will perform a backpurge on the reagent(s) selected from the list. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009...
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Page 67: Using The Change Bottle Command
The Change Bottle window will appear. Click Next to begin the Change Bottle procedure. The Liberty will clear the line to the bottle, and then vent the pressure to the bottle. The Change Bottle window will indicate it is safe to remove the bottle. Remove the old bottle from the system and connect a fresh bottle. -
Page 68: Performing A Backflush
Maintenance screen. Performing a Backflush NOTE For detailed instructions on performing a backflush, see the Liberty Maintenance Procedures manual, PN 600119. Remove all bottles and dip tube filters from the positions to be backflushed. Connect empty bottles to all positions to be backflushed. -
Page 69: Performing A System Check
Performing a System Check A System Check is a basic diagnostic test of the Liberty’s flow paths and valves. When a System Check is run, a PDF containing information about the Liberty as well as the results of the various tests is generated. -
Page 70: Revision 5 • October
OK to continue. The Liberty will perform an unfiltered drain on the reaction vessel to ensure it is empty, and then it will purge all liquid from all manifolds. This process will take approximately 5 minutes. -
Page 71: Sample System Check File
(Normally Closed/Normally Open) RV2: -0.1/-0.1 RV4: 0.0/-0.1 RV7: 0.0/0.0 -0.1/0.0 RV3: -0.1/-0.1 RV6: 0.0/0.0 -0.1/-0.1 Valve RV7(3.1, 3.7) Failure: Valve did not open Please email this file to: service@cem.com ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 72: Volume Calibration Tab
In addition, the Volume Calibration tab allows for the calibration of amino acids at large scale. For additions of more than 11 mL, the Liberty switches from a sample loop to a timed addition to reduce the time required for each addition. - Page 73 Liberty. CAUTION Cleavage should only be calibrated if Boc chemistry is being performed on the Liberty. After performing a cleavage volume calibration, perform a reaction vessel neutralization by clicking Neutralization on the Cleaning tab of the Maintenance screen.
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Page 74: Importing And Exporting Volume Calibration Values
Click the Filtered Drain button to empty the reaction vessel. NOTE When calibrating Add DMF to Resin or Add DCM to Resin, the Liberty will add reagent to a centrifuge tube connected to position 1 on the Resin Manifold. One the reagent has been added, remove the centrifuge tube and transfer the liquid to a graduated cylendar to accurately measure the delivered volume. -
Page 75: Performing A Large Scale Calibration
From the Volume Calibration Tab, click on the Large Scale Addition Tab. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... - Page 76 Enter the delivered volume in the Prime Volume box, and then click the second Add button. The solvent will be automatically drained from the reaction vessel. Following the filtered drain, the Liberty will add a delivery volume of DMF to the reaction vessel (approximately 20 mL). ™...
- Page 77 Enter the delivered volume in the Delivered Calibration Volume box, and then click Calibrate. Two values will appear below the Calibrate button: New Rate and New Prime Volume. Click Save to save the new calibration values. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009...
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Page 78: Sensor Calibration Tab
Sensor Calibration Tab The Sensor Calibration tab allows for the calibration of the sensors used to monitor the addition and transfer of reagents in the Liberty. Sensor calibration should be performed monthly as part of routine maintenance. Performing a Sensor Calibration... - Page 79 Click Calibrate to the begin the sensor calibration procedure. A series of warning boxes will pop up to ensure sufficient DMF is loaded on the Liberty for the test. Verify there is sufficient DMF in the Main Wash bottles and click OK.
- Page 80 A window will pop up suggesting running a window. Click the Test Sensors button to begin a Sensor Test. NOTE For information on performing a Sensor Test, see Test Sensors, p. 91. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009...
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Page 81: Importing And Exporting Sensor Calibration Values
Pressure Calibration Tab The Pressure Calibration tab allows for the calibration of the pressure sensor on the Liberty. Pressure calibration is not necessary for routine maintenance; a calibration should only be done as part of a troubleshooting protocol as advised by CEM Service. -
Page 82: Performing A Pressure Calibration
Click Yes to backpurge the system before calibrating. NOTE Put empty bottles on all positions before performing a backpurge. Adjust the pressure on the main pressure regulator in the Liberty to 16 psi, and then click OK to continue the calibration. ™... - Page 83 The Liberty will vent the pressure on the entire system to get a zero pressure reading, and then apply pressure to get a main pressure reading. Look at the pressure regulator on the Liberty and enter the current reading. Click OK to continue the calibration.
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Page 84: Section 5: Advanced Features
Select a scale from the Scale pull-down menu. Click on the cycle next to the an amino acid and select the desired cycle from the pull-down. Click OK to save the new default cycles. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 85: Options Menu
• Automatic Leak Check RV at Start: When this option is enabled, the Liberty will perform a leak check of the reaction vessel before starting the first method in the queue. This option is enabled by default. • Automatic... - Page 86 The 125 mL reaction vessel must be used for syntheses above 0.25 mmol. Using the 35 mL reaction vessel for large syntheses will result in overfilling of the vessel, loss of product, and possible damage to the instrument. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009...
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Page 87: Defaults Tab
The Run History tab is used to select the format for naming the folders into which run history files are saved. Folders can be named in either American (Month-Year) or European (Year-Month) format. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 88: Test System Screen
The Test System screen contains a number of diagnostic tests that can be used to troubleshoot the performance of the Liberty. The Test System screen is accessed by clicking the Maintenance button, selecting Maintenance, and then clicking the Test System button from the Cleaning tab of the Maintenance menu. -
Page 89: Pressure Adjustment
The pressure reading will be displayed in real time. Adjust the regulator until the reading is between 15 and 17 psi. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 90: Low Pressure Adjustment
The pressure reading will be displayed in real time. Adjust the regulator until the reading is between 2.5 and 4.5 psi. Contact CEM Service for help adjusting the low pressure regulator. Leak Check The Leak Check category contains tests to ensure none of the manifolds on the system are leaking. -
Page 91: Test Rotary Valves
The Liberty will purge all manifolds, and then apply pressure to the manifold to be tested. The pressure will be monitored for a set amount of time, during which the current drop in pressure at the manifold being tested will be displayed in the status box. -
Page 92: Internal, Nitrogen, And Liquid Delivery Tests
Delivery, and Liquid Delivery. Each category corresponds to a specific flow path within the Liberty, and each contains individual tests of each valve in that path. The delivery tests are intended to test the function of each valve on the system. -
Page 93: Performing A Delivery Test
Test window (or click Test to test all valves within the category). The Liberty will vent all pressure from the lines. The valve will be closed and the line pressurized, then the nitrogen turned off. The Liberty will wait to see if there is a decrease in pressure. - Page 94 Verify the DMF supply and that the waste container is not full, then click OK. The Liberty will purge the lines. The sensors for the first test will be displayed in the status window. The Liberty will fill the line with DMF. As each sensor detects liquid, the corresponding indicator in the status window will turn bright green.
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Page 95: Reagent, Amino Acid, And External Amino Acid Addition
To perform an Addition Test: Disconnect the sprayhead line from the manifold on the front of the Liberty. Connect a piece of 1/8” OD tubing (PN BR199116) to the manifold using a nut (PN 167810) and yellow ferrule (PN 164315). -
Page 96: Leak Check Reaction Vessel
CEM Service.) Flow Performance The Flow Performance test is intended to verify there are no restrictions in the lines of the Liberty by testing the rates of nitrogen flow through all lines and manifolds. Typically, this test is only performed on the advice of CEM Service to aid in diagnosing a problem. -
Page 97: Diagnostics Screen
The Diagnostics Screen contains a number of reports and manual controls that are not intended for normal use. In general, the Diagnostics screen should only be used under the advice of a trained CEM Service Technician. Commands Tab The Commands tab allows for the manual execution of all system commands. In addition, the Read Discover Errors button will detect any firmware errors in the Discover. -
Page 98: Valves Tab
The Rotary Valves are controlled by selecting the desired position from the pull-down box and then clicking the button corresponding to that valve (1 for Rotary 1, 2 for Rotary 2, 3 for Rotary 3). Status Tab The Status tab contains diagnostic information about the current status of the Liberty. ™ Liberty Automated Microwave Peptide Synthesizer 600178 •... -
Page 99: Delay Times Tab
Enter the new delay time in the Delay Time (sec) box on the right. Click Update to save the new delay time. CAUTION Do not change a delay time without consulting with a trained CEM Service Technician. Incorrect delay times can result in poor synthesis quality and instrument malfunction. -
Page 100: Section 6: Troubleshooting
Leak Check • Verify the quick disconnect on the drain line is tightly secured • If the vessel still fails the Leak Check, contact CEM Service ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 101: Tips For Recovering From Errors
If an error occurs on an Add Activator or Add Activator Base step, perform a filtered drain and reswell the resin as above, except restart with the Add Amino Acid step. ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 102: Section 7: Spare Parts And Consumables
Consumables Reaction Vessel Parts Part Number Name Description Picture Standard reaction vessel 30 mL Reaction attenuator used for the Liberty 516030 Vessel with the 30 mL and 125 mL Assembly reaction vessels Modified reaction vessel 10 mL Reaction attenuator specifically... -
Page 103: Filters
Picture Optional steel keg with 20 L Solvent bladder for use as 20 L DMF 908515 (not pictured) reservoir (includes keg and all Keg Kit necessary tubing) ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 104: Bottles
(bag of 24) Bottle 50 mL Standard 50 mL centrifuge Polypropylene tube used on resin, product 167150-M (not pictured) and external amino acid Centrifuge manifolds (set of 15) Tube ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 105: Bulk Tubing And Fittings
PEEK nut for 3/16” tubing (PN Ferrule 167315) PEEK fitting used for 3/16” to 1/8” 167275 connecting 3/16” OD tubing to (not pictured) Fitting 1/8” OD tubing connections ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 106: Bottle Tubing Assemblies
(see 167963) 167688 Assembly, connect an external cleavage bottle to the manifold Purple DMF TEE Tubing used to connect two 167971 DFM bottles to the manifold Assembly ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 107: Bottle Caps
Cap (Orange) solution Teflon bottle cap for use with GL-45 Bottle 167575 (see 167560) an external bottle of cleavage Cap (Purple) solution ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 108: Dip Tubes
174000 (not pictured) O-Ring valves (PN 167855) O-ring uses to seal the top Reaction 167731 (not pictured) of the reaction vessel to the Vessel O-Ring attenuator assembly ™ Liberty Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009... -
Page 109: Valves And Valve Wiring
Valves and Valve Wiring Part Number Name Description Picture Main 2-way valve used on the 2-Way Valve 167850 Liberty 2-way valve used for Teflon 2-Way 172088 deprotection (LE9) and Valve capping (LE7) liquid valves 3-way valve used to pressurize 167855... -
Page 110: Liquid Sensors
Part Number Name Description Picture Teflon 3-way valve used on 3-Way Valve the Liberty used for positions (Teflon, long 167410 M3 and M5 (integrated wiring- no additional wiring assembly wire) required) Large 3-way valve used on Large 3-Way the Liberty (integrated wiring-... -
Page 111: Waste Container
Cable that connects the level 243155 (not pictured) Wire Harness sensor to the Liberty Waste Tubing Tubing assembly that connects 167970 (not pictured) the waste cap to the Liberty Assembly Accessories and Tools Part Number Name Description Picture Reaction Stand used to hold the... -
Page 112: Computer Accessories
(PN 167810) Tool uses for connecting 50 Centrifuge mL centrifuge tubes to the 167875 (not pictured) resin and product manifolds of Tube Tightener the Liberty Chemical Safety labels for all reagent 167955 (not pictured) bottles Bottle Labels Discover Spill Large spill tray to protect the... -
Page 113: Circuit Boards
Circuit Boards Part Number Name Description Picture 576020 CPU Board (not pictured) Main CPU board for the Liberty Valve Valve controller boards for the 576006 Controller (not pictured) Liberty Board Sensor controller board for the 576040 Sensor Board (not pictured) -
Page 114: Revision 5 • October
C-terminal Acid Purple, 104 Red, 104 Activator Addition Test, 92 Bottle Tubing Assembly Calculator, 41 Black, 103 Loading onto Liberty, 47 Blue, 103 Preparing Solution, 45 DMF TEE, 103 Standard Concentration, 44 Green, 103 Orange, 103 Activator Base Addition Test, 92... - Page 115 Contact Information, 10 Depressurize Command, 62 Technical Support, 9 Deprotection, 58 Centrifuge Tube, 101 Calculator, 40 Loading onto Liberty, 47 Change Bottle Command, 47 Preparing Solution, 46 Circuit Boards Diagnostics Screen, 94 CPU Board, 110 Pressure Board, 110 Dichloromethane, 49...
- Page 116 . See Inline Filters Filters, Inline Multi-Step, 24 Standard, 24 Microwave Power, 25 Leak Check, 85 Leak Test, 64 Liberty Automated Microwave Peptide . See Neutralization Command Reaction Synthesizer, 15 Vessel: Neutralization Components and Parts, 17 NOTE (Description), 12 System Requirements, 13 N-terminal Acetylation, 36 .
- Page 117 Temperature Probe, 17 Resin . See Test Sensors Sensor Test Calculator, 39 Test System Screen, 64 Loading onto Liberty, 49 Substitution, 36 Transfer from Resin Tube to RV Command, 63 Trifluoroacetic Acid, 42 Resin Return Command, 63 . See also...
- Page 118 Waste Full Error, 97 Waste Full Indicator, 21 Waste Sensor, 108 Liberty ™ Automated Microwave Peptide Synthesizer 600178 • Revision 5 • October 2009...