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413457 Isolera Dalton Getting Started Guide

1. To perform a mass detector function test 1 Inthe chemistry mode select the Setup tab in the right hand panel 2 Select the Mass Detector tab 3 Press Signal or Baseline in the Function Test field The Mass Detector Function Test dialog opens 4 Press gt Positive and monitor the results Results marked in green indicate proper function If running a baseline test verify that the signal and scans are stable and uninterrupted for the TIC and spectrum graphs This may take up to 20 minutes to achieve If running a signal test verify that you have a strong and clear peak profile at 65 1 0 7 m z 5 When you have collected enough data to determine whether the mass detector is working properly or not in the positive ionization mode press Stop 6 Press gt Negative and monitor the results If running a baseline test verify that the signal and scans are stable and uninterrupted for the TIC and spectrum graphs This may take up to 20 minutes to achieve If running a signal test verify that you have a strong and clear peak profile at 75 0 20 7 M Z 7 When you have collected enough data press Stop 8 To close the dialog press Close Note If the mass detector is not working properly proceed to the Troubleshooting section on page 19 for further instructions or contact Biotage 1 Point Support Prepare Isolera One or Isolera Four for a Run Load the Chromatography Solvents Note Ensure that no foreign
2. Dalton Mass Detector Flush the Mass Detector Tubing To prevent blockage of the mass detector when cancelling a run we recommend that you empty the internal tubing of the previous solvent using the flush feature 1 Verify that the waste reservoirs are in place see the Verify the System Setup section on page 9 2 Inthe chemistry mode select the Setup tab in the right hand panel Maintenance Select the Mass Detector tab Select the Makeup Solvent A text box in the Flush Tubing and Mass Detector field and select the makeup solvent to be used 5 Select the Isolera Solvent B text box and select the Isolera solvent to be used 6 Press Start Flush and wait for the system to finish the flush A status field and progress bar in the right hand panel indicates the progress Air Flush Instrument Solvents Main Mer akeup Solvent Neutral P Start Prime 0 6 bar Skip Warm Up Makeup Solvent gt Select the solvent to be used when priming the Resume makeup pump See and Nin the image Na Skip Vacuum Makeup Solvent my Makeup Solvent A Positive Neutral Help ae Negative _ solera Solvent B Neutral p Start Flush Baseline Signal Figure 17 At the Mass Detector tab it is possible to flush the mass detector and Isolera Dalton Nanolink tubing Main Menu Last Calibration Calibrate Help JV Detecto Mass Detector Last Calibration Intensity
3. Calibrate Soa Last Check Valve Release Q Restore Configuration Last Restore Last Backup a lt Back Up 34 Back Up oS Restore 25 Restore sa Last Collect Valve Clean Release Clean Check Valves Collect Valve Performed Runs Performed Runs Since Last Reset 0 0 Reset Last Calibration Active Splitter Switches 2 e z 3 Reset Active Splitter Calibrate Replace spraychip Replace vac chip ern Figure 18 At the Maintenance tab in the system mode it is possible to calibrate the mass detector clean or replace a vac chip or spra chip and reset the counter for the active splitter switches after replacing the rotor seal and stator face assembly 15 Maintenance Calibrate Isolera Dalton Mass Detector If the mass accuracy is not within 0 7 m z the mass detector may need to be recalibrated Required The calibration kit supplied with the mass detector P N 413715 at least 500 ul filtered calibration solution see step 1 below and at least 500 ul filtered cleaning solution 1 1 methanol water 1 Prepare the calibration solution i Mix50 ml of HPLC grade water with 50 ml of HPLC grade 2 propanol ii Dissolve 100 mg of sodium formate for HPLC 299 0 Fluka 17841 in the solution iii Filter the sodium formate solution through a 0 22 um PTFE or nylon based syringe filter iv Mark the solution with one month expiry date Press Main Menu in the right hand panel Pres
4. Main Menu Air Flush Mass Detector Solvent 1 olvent Reservoirs ml Re Capacity Select the solvent connected to solvent channel ST n Hexane 4000 0 6 bar Solvent 2 Capacity Ethyl acetate 4000 Name Strength Turn Solvent 3 Capacity 2 Propanol 0 82 Lamp Off 4000 p Capacity Acetonitrile 4000 Cyclohexane Dichloromethane ste Reservoir ml Capacity gt Help 4000 Resume Mass Detector Running At the Instrument Solvents tab you assign the solvents used in the method to the solvent inlets on Isolera One or Isolera Four 11 12 Prepare and Run a Purification Prime the Solvent Inlets on Isolera One or Isolera Four Prime the solvent inlets on Isolera One Four to remove any air bubbles from the pump and the solvent inlets by flushing them with solvents or empty the solvent inlets of solvents used in the previous purification and fill them with new solvents Warning Never prime Isolera One Four without a cartridge mounted on the system or without the cartridge s inlet and outlet tubing coupled together To avoid leakage check all tubes and fittings before priming Note All solvent inlets on Isolera One Four must be primed with solvent to achieve the specified pump performance 1 Ensure that a sufficient quantity of the solvents you want to use is present in the solvent reservoirs and the waste reservoir s has have sufficient capacity for the prime Select the Setup tab i
5. Weight Power Max Power Consumed Altitude Temperature Relative Humidity Pollution Degree Mass Detector Nitrogen Gas Fuses Installation Description Dalton Mass Detector 32 kg 70 5 Ibs Dalton Nanolink 10 kg 22 5 Ibs Isolera One Four 30 35 kg 66 77 Ibs depending on system configuration Line voltage 100 to 240 V AC 10 Line frequency 50 60 Hz Isolera One Four and Isolera Dalton Nanolink must be connected to a common ground which is achieved by using the same power outlet Dalton Mass Detector 320 VA Dalton Nanolink 130 VA Isolera One Four 200 VA Operation up to 2000 m Operation 15 C to 30 C Storage of Dalton Mass Detector 10 C to 50 C Operation 40 to 80 non condensing for temperatures up to 30 C Storage of Dalton Mass Detector 0 to 80 non condensing Dalton Mass Detector 2 Pressure 2 to 6 bar 29 to 87 psi Purity 99 9 Tubing Only use 1 4 OD tubing in stainless steel or PTFE to connect the mass detector to the gas supply Five meters of PTFE tubing is supplied with the mass detector If a fitting for conversion to 1 4 OD is necessary the fitting must be in stainless steel or PTFE Dalton Nanolink T2A 250 VAC 2 required Isolera One Four T4A 250 VAC 2 required Move or Disconnect Isolera Dalton Mass Detector and Isolera Dalton Nanolink If you want to use Isolera One Four without the mass detector or move the system within the l
6. 32 kg 70 5 Ibs Two persons are required when lifting the detector e Follow regional safety practices when moving the system Note Isolera Dalton Nanolink weighs 10 2 kg 22 5 lbs 1 Verify thatthe system has been shut down and the power cords disconnected from the power outlets see page 5 2 Verify that the mass detector and Isolera Dalton Nanolink have been disconnected from Isolera One Four see page 6 3 Carefully lift Isolera Dalton Nanolink and place it on a trolley Place the Isolera Dalton Nanolink tray on the trolley Carefully lift the mass detector and place it on a trolley Two persons are needed 6 Move the trolley s with the mass detector Isolera Dalton Nanolink tray and the rest of the equipment to the new location 7 Move Isolera One Four to the new location by carefully reading and following the instructions in the Moving an Isolera System section in the Isolera Installation and Safety document P N 411828 Note Do not turn Isolera One Four on until you have connected the mass detector and Isolera Dalton Nanolink 8 Carefully lift the mass detector and place it on the left side of Isolera One Four Two persons are needed g Place the tray on top of the mass detector with the drain tube to the back 10 Place the drain tube in a reservoir or on the Isolera leak tray if using Biotage Leak Detector Ensure the tube and reservoir if used is visible from the working position
7. Torn Door Spray Current Establ Acquiring Yes 8 00x 107 100 1072 Closed 0 00 0 20 0 40 1 20 Spectrum m z 130 170 210 250 290 330 370 410 450 490 530 570 610 650 690 730 770 gt Negative E Stop Close Positive Figure 13 After installation long term storage or for troubleshooting purposes you are recommended to perform a mass detector function test Perform a Mass Detector Function Test After installation long term storage or for troubleshooting purposes you are recommended to perform a mass detector function test There are two function tests available Baseline Used to monitor the complete mass range 50 to 800 m z and the status of the mass detector such as pressure vacuum levels and spray current In this test the background noise is observed and can be used to discover contamination peaks Isolera Dalton Getting Started Guide Biotage 2015 Signal Used to monitor a specific peak and mass range the positive range is 50 to 80 m z and the negative is 60 to 90 m z and the status of the mass detector such as pressure vacuum levels and spray current In this test a lower vac chip voltage than what is normal during arun is applied which allows methanol to create cluster ions visible at 65 1 m z positive mode and 75 0 m z negative mode Observe the intensity and abundance during the test a well working system should have a strong and clear peak profile in both positive and negative mode
8. may indicate leakage or malfunctioning check valves in Isolera Dalton Nanolink Please contact Biotage 1 Point Support Higher than 6 5 bar this may indicate a microfilter blockage Replace the microfilter as described in the High Makeup Flow Pressure dialog that appears or on page 18 If this does not solve the problem the stator face assembly may need to be replaced see page 18 Ifthe mass detector vacuum pressure is outside the specifications see below this may indicate a vac chip blockage or vacuum leakage in the mass detector Clean or replace the vac chip as described on page 16 or contact Biotage 1 Point Support 1G ion guide vacuum approx 1x 10 Torr in running mode and 1 x 10 Torr in standby mode AQ analytical quadrupole vacuum lt 5 x 10 Torr This value will decrease the longer the system is left under vacuum Troubleshooting Leaks Warning Do not wipe away any excess solvent from the cartridge surface as the process of wiping can generate additional static charge Ifa leakage is detected immediately turn off the Isolera system and disconnect the power cord from the power outlet If the leakage is clearly located to the connections or the external tubing of Isolera Dalton Nanolink replace the relevant tubing Only use spare parts and accessories from Biotage If the needle port for direct injection is leaking during sample injection replace it P N 413487SP If the needle port fo
9. placement and leakage collection Front Panel A Needle port for direct injection B External check valve for direct injection C Tubing to the active splitter D Tubing from the active splitter E Tubing orange from the makeup pump to the active splitter F Filter unit with microfilter G Tubing from Isolera One Four 140 cm H Tubing to Isolera One Four 120 cm with adapter Tubing to the SFI inside the mass detector Figure 5 The front panel of Isolera Dalton Nanolink Right Side Panel Solvent inlets positive N neutral and negative Waste outlet Check valve release port N A Figure 6 The right side panel of Isolera Dalton Nanolink Rear Panel From left to right Power switch Power inlet fused 100 to 240 V AC 10 Isolera One Four and Isolera Dalton Nanolink must be connected to a common ground which is achieved by using the same power outlet Fan USB port type B for connecting the unit to Isolera One Four Figure 7 The rear panel of Isolera Dalton Nanolink Isolera One and Isolera Four Please refer to the Isolera User Manual P N 411829 or the system s online Help for more information on Isolera One and Isolera Four and their specific functions Isolera User Documentation The following Isolera user documentation can be downloaded from the system Isolera Installation and
10. service or moved to another location Note Before the system is shipped to the customer its internal tubing is flushed with methanol Isolera Dalton Mass Detector and Isolera Dalton Nanolink and 80 ethanol in deionized water Isolera One Four and then emptied Site Requirements Before the system is installed by an authorized Biotage service engineer the installation site should be prepared as follows Requirement Description Location A laboratory fume hood with capacity to handle leakage of solvents used and provide and suitable airflow to prevent the build up of flammable vapors Note that if an internal system leakage occurs the maximum leakage volume is determined by the size of the used solvent reservoirs and the flow rate is determined by the used method max 200 ml min External fire protection should be installed according to local regulations for equipment operating unattended Bench Space Dalton Mass Detector W x D x H 355 mm x 560 mm x 255 mm 14 x 22 x 10 Dalton Nanolink 354 mm x 525 mm x 206 mm must be placed on the tray on top of Dalton Mass Detector Isolera One Four W x D x H 355 577 mm x 497 mm x 596 mm 14 22 7 x 19 6 x 23 5 The width is dependent on the number of collection trays one two At least three centimeters one inch of space should be maintained between the rear panel of Isolera One Four and other objects to allow proper ventilation Requirement
11. which is achieved by using the same power outlet Turn on the system as described on page 10 and perform a mass detector function test as described on page 10 Note In case of communication problems with the mass detector try to resolve the problem and then press Test Communication at the Detector tab in the system mode to verify that the problem has been resolved Isolera Dalton Getting Started Guide Biotage 2015 System Setup General Use Recommendations Always use methanol of LC MS grade and purified water for the makeup solvents on Isolera Dalton Nanolink See Load the Makeup Solvents on page 10 Always use a clear and filtered 0 5 um or less pore size sample for analysis to avoid clogging the system Always equilibrate the system and the cartridge before arun to avoid clogging the system Always flush the mass detector and Isolera Dalton Nanolink tubing with neutral solvent makeup solvent and methanol or similar Isolera solvent after using DCM or before shutting the mass detector down or leaving it for more than 12 hours This prevents e g blockages in the spraychip and vac chip See Flush the Mass Detector Tubing on page 15 for instructions Never allow the waste outlet tube at the front of the mass detector to become immersed in the waste liquid Werecommend that the mass detector is only shut down for long term non usage and or when it is to be moved or to replace externa
12. Detector Ensure that the drain tube and reservoir if used is visible from the working position to detect leakage Verify that any refitted tubes are assembled correctly To ensure proper sealing for tubing connected at the front of Isolera Dalton Nanolink it is important to orient the ferrule with the tapered portion of the ferrule facing away from the nut Carefully place the ferrule inside the fitting before fastening the nut Figure 10 Ferrule with the tapered portion facing away from the nut Verify that the tubing is inserted correctly Tubes should be inserted all the way and tube fittings nuts tightened Use caution when finger tightening fittings to prevent stripped threads or crushed ferrules Isolera One and Isolera Four Verify that each waste outlet tube on the right hand side is inserted into a waste reservoir Verify that the drain tube for the solvent tray connected at the rear of the system is inserted into a separate waste reservoir Verify that Isolera One Four is set up correctly see the Isolera Installation and Safety P N 411828 Verify that any refitted tubes are assembled correctly If using flangeless tubing please notice that proper sealing is only achieved with the ferrule oriented with the tapered portion of the ferrule facing toward the nut The ferrule should be placed near the end of the tube If using super flangeless tubing ensure the ferrules are fit
13. Isolera Dalton Getting Started Guide je an we mu PRET 5 _ In s r Re LE ol gt taka nex f omase EE Sow As rrouce te aha D Cube i Cie Bor Biotage MANAN Biotage nt e Biotage il Microsaic Biotage Contents Isolera Dalton Getting Started Guide CONTENTS 1 Intended Use and Safety 2 System Overview 5 Installation 9 System Setup 10 Prepare and Run a Purification 15 Maintenance 19 Troubleshooting 20 Hints and Tips 21 General Information Isolera Dalton Getting Started Guide Biotage 2015 Intended Use and Safety Intended Use Isolera Dalton System Isolera Dalton System from Biotage is intended solely to detect fractionate and analyze chemical mixtures using flash chromatography and electrospray ionization mass spectrometry or light absorbance The system must be operated in a laboratory environment by trained professionals The system is not designed to be operated in a potentially explosive atmosphere It is the responsibility of the customer to classify zone their particular environment in order to verify that it meets the requirements of a non hazardous area with regards to potentially explosive atmosphere All operations must be performed According to the user documentation delivered with the system According to instructions available at www biotage com According to instructions provid
14. OK iv If your account is password protected the Password dialog opens Enter your password and press OK v Select the Detector tab vi Select the Connect at Startup text box in the Mass Detector field and select Yes The Restart Required dialog opens vii Press OK 4 Shut down Isolera One Four i Press Main Menu in the right hand panel ii Press Shut Down in main menu and then Yes to confirm iii When the message It is now Safe to turn off the system appears on the screen turn off Isolera One Four The power switch is located underneath the touch screen D 10 11 Disconnect the tube connected between the fraction collector and the flow cell from the flow cell s upper port A and connect it to the extension connector B on the tube connected to the To Isolera port on Isolera Dalton Nanolink Connect the tube connected to the From Isolera port on Isolera Dalton Nanolink to the flow cell s upper port A Connect the two communication cables see the scheme above Connect the filter unit C to Isolera Dalton Nanolink Connect the mass detector to a nitrogen gas supply with a pressure of 2 to 6 bar and a purity of 99 9 Only use clean Stainless steel or PTFE tubing and fittings for the nitrogen gas line to avoid contamination Connect the mass detector and Isolera Dalton Nanolink to the mains supply Isolera One Four and Isolera Dalton Nanolink must be connected to a common ground
15. Safety P N 411828 Isolera User Manual P N 411829 Isolera Quick Guide P N 411830 Isolera Safety Translations P N 412861 Isolera Dalton Getting Started Guide this document P N 413457 Isolera Dalton System Care Guide P N Ul320 To download the documents from the system connect a USB memory device to the USB port located underneath the touch screen press Help and then press Export User Documentation You can download the latest versions of the documents at www biotage com If you have problems downloading please contact your local Biotage representative Isolera Dalton Getting Started Guide Biotage 2015 Installation Warning e Isolera Dalton System shall be unpacked and installed by an authorized Biotage service engineer e The total weight of the packages are approx 50 kg 110 Ibs for Isolera Dalton Mass Detector 20 kg 44 Ibs for Isolera Dalton Nanolink and 42 46 kg 93 102 Ibs for Isolera One Four Use Suitable lifting equipment when moving the packages Follow generally accepted safety practices when handling and moving shipping boxes and containers Delivered Items Check the delivery against the shipping documentation to ensure that you have received everything If any part of the order is missing contact Biotage 1 Point Support Note We strongly recommend that the boxes and packing materials are kept by the customer in case the system needs to be returned for
16. a 3D absorbance spectrum for the whole detector range and TLC data if entered and 2 a fraction report Shut Down the System We recommend that you keep the mass detector turned on for regular use For longer periods of inactivity or storage please follow the instructions in the Shut Down the System Not for Daily Operation section on page 5 The instructions below describe the procedure for shutting down after a working day 1 If the mass detector is not planned to be used for 12 hours or more always flush the mass detector and Isolera Dalton Nanolink tubing with neutral solvent makeup solvent and methanol or similar Isolera solvent to e g prevent blockages in the spraychip and vac chip For instructions see the Flush the Mass Detector Tubing section on page 15 2 3 Turn off Isolera One Four i Press Main Menu in the right hand panel ii Press Shut Down in main menu and then Yes to confirm The Mass Detector dialog opens iii If you want to vent the mass detector to atmospheric pressure press Vent Otherwise press Leave On iv When the message It is now safe to turn off the system appears on the screen turn off Isolera One Four The power switch is located underneath the touch screen Turn off Isolera Dalton Nanolink using the power switch located at the rear Isolera Dalton Getting Started Guide Biotage 2015 Maintenance Please also refer to the Isolera Dalton Syst
17. aboratory or between laboratories in the same building follow the applicable instructions below Shut Down the System Not for Daily Operation Note Only use this procedure to shut down the system when you want to 1 disconnect the mass detector to use Isolera One Four without it or move the system 2 replace external tubing or 3 clean the exterior of the system 1 Inthe chemistry mode select the Setup tab in the right hand panel 2 Select the Mass Detector tab Installation 3 10 11 Clean the mass detector and Isolera Dalton Nanolink tubing by flushing it with neutral solvent makeup solvent and methanol or similar Isolera solvent see Flush the Mass Detector Tubing on page 15 Empty the makeup solvent inlets by removing the inlets from their reservoirs and then priming them with air See Prime the Makeup Solvent Inlets on page 10 Empty the tubing between Isolera One Four and Isolera Dalton Nanolink by performing an air flush i Select the Air Flush tab ii If you are using a system with four cartridge positions select the Channel text box and select 1 ili Select the Cartridge Type text box and select a cartridge e g SNAP KP Sil 10g Note The cartridge does not have to be mounted on the system iv For the pump to work properly a small amount of solvent has to be used Select the Solvent text box and select the desired solvent v Ensure that a sufficient quantity of the sel
18. al guidelines on laboratory safety procedures 1 If necessary empty the cartridge of remaining solvents and pressure by using the air flush and purge features at the Setup tab For instructions press Help 2 If you are using a system with four cartridge positions and the system is processing press Pause 13 14 Prepare and Run a Purification 3 Unload the cartridge To avoid leakage plug the cartridge s inlet and outlet fittings and couple the inlet and outlet tubes together 4 Unload the rack s used by the run Allocated racks are listed at the Allocated heading at the Status tab 5 To clear the cartridge and rack positions in the software press Remove 6 If necessary empty the waste reservoirs 7 To resume processing of queued runs see step 2 above press Resume Access Result Records Purifications that are processed on the system are stored as individual records in the system s database and can be found at the Results tab For more information refer to the Isolera User Manual or press Help to access the online help Result Selection Report Setup Fractions Report Main Me Lars 2013 May 24 13 50 gt Resume Mass Detector Running 279 2 m z Help 80 140 Gradient Figure 16 Two result reports are available for each purification 1 an archive report with the selected spectrogram from the mass analysis if available purification details a chromatogram
19. ass detector in its installed location via access through the door 99 System Overview Front Panel A Power switch for turning on the mass detector B Door Only open the door for maintenance purposes when the system is not processing see Safety Interlock above C High voltage port max 1500 V max 5 mA for connecting the split flow interface SFI or the direct flow interface DFI Biotage Figure 3 The front panel of Isolera Dalton Mass Detector Rear Panel The following items at the rear panel are relevant when the mass detector is connected to Isolera One Four A Nitrogen gas port B RS232 port for connecting the syringe pump included in the calibration kit C 4xUSB ports One is for connecting the mass detector software dongle D Ethernet port for connecting the mass detector to Isolera One Four E Pump exhaust with sound silencer F Power switch and power inlet 100 to 240 V AC 1096 Figure 4 The rear panel of Isolera Dalton Mass Detector System Overview Isolera Dalton Nanolink Basic Components Active splitter with an integrated mass rate attenuation device Makeup pump Needle port for direct injection Tubing to and from Isolera One Four and tubing with a filter to the mass detector Solvent inlets for makeup solvents for neutral and for negative and positive ionization Tray for safe assembly solvent reservoir
20. ater 9 1 7 0 5 concentrated ammonium hydroxide in methanol water 9 1 Prime the Makeup Solvent Inlets We recommend that a makeup solvent inlet is primed each time the makeup solvent is replenished 1 Verify that a waste reservoir is connected to the WASTE port on the right hand side of Isolera Dalton Nanolink 2 Inthe chemistry mode select the Setup tab in the right hand panel 3 Select the Mass Detector tab Select the Makeup Solvent text box in the Prime Makeup Pump Inlet Tubing field and select the makeup solvent to be primed positive negative or neutral 5 Press gt Start Prime A status field and progress bar in the right hand panel indicates the progress 6 Repeat steps 4 to 5 for the other two solvents Air Flush Instrument Solvents Makeup Solvent Neutral gt Start Prime Enc usn Jping and 155 Detecto 0 6 bar Skip Warm Up p Resume Mass Detector Skip Vacuum Stabilization Help Method Makeup Solvent Select the solvent to be used when priming the makeup pump See and Nin the image Makeup Solvent Positive Negative Neutral Makeup Solvent A Neutral Isolera Solvent B Figure 12 At the Mass Detector tab it is possible to prime the makeup solvent inlets and flush the mass detector and Isolera Dalton Nanolink tubing Mass Detector FL action est saselin ass Detector Status ass Detector Spra Status At Vacuum AQ Vacuum Torr IG Vacuum
21. c chip blockage may be indicated by 1 a low pressure reading of the ion guide IG vacuum or 2 a low mass detector signal when running a mass detector function test signal Clean or replace the vac chip Required Powder free gloves and a vac chip P N 413712SP You also need the pair of tweezers flat headed screwdriver Allen key and dust cover supplied with the mass detector 1 Press Main Menu in the right hand panel Press System The Select User dialog opens Select your user name and press OK If your account is password protected the Password dialog opens Enter your password and press OK Select the Maintenance tab ON Ul Press Replace vac chip in the Mass Detector field and follow the instructions appearing on the screen Maintenance Maintenance of Isolera Dalton Nanolink Leakage at the Direct Injection Port If the needle port A for direct injection is leaking during sample injection replace it P N 413487SP If the needle port A is leaking when the Isolera pump is running the check valve C may need to be cleaned or replaced To clean unscrew the direct injection port assembly see Figure 20 below and inject a cleaning solution that is appropriate for the residues using the 250 ul syringe supplied with Isolera Dalton Nanolink If necessary unscrew and clean the check valve C using an ultra sonic bath If this does not solve the problem replace the check valve P N 413480SP Note Ensu
22. city 9 When you have finished loading the sample press Close and reconnect the cartridge inlet tubing to the cartridge s inlet 10 Start the gradient run by pressing Gradient While the purification is running one graph displays the programmed gradient and the other a dynamic chromatogram The signals for the selected wavelength s and or m z ratios are displayed in the chromatogram An absorbance spectrum for the whole UV detector range can be viewed in the gradient view by pressing the Show button The gradient is then displayed in the chromatogram 11 When the run is finished press Show Report to view and or print a report It is also possible to save the report as a PDF file on a connected USB memory device Main Menu radient 270 ml 125 ml 10C Est Finish 14 05 80 Zoom 50 Drag 40 Scroll 20 Rail o Length 6 m 279 2m z m 223 0 m z E all 1703 mw 195 2 m z sal 14 bar 50 ml min Turn Lamp Off 5 UV Zero Hold Collect R nm 200 250 300 350 400 450 500 550 600 650 700 750 800 Show New Load Sample D Gradient a Stop Edit Remove Figure 15 While a purification is running the programmed gradient and a dynamic chromatogram are displayed The chromatogram can be magnified dragged to the desired position etc Unload a Purification Warning Handle chemical and liquid waste according to the Safety Data Sheets and local nation
23. ct Ion M 59 Acetic acid M CH3COO M 35 37 Chlorinated solvent M CIT M 18 Ammonia M NH4 M 23 Sodium salt M Na M 39 Potassium salt M K M 42 Acetonitrile M CH3CNH M 33 Methanol M CH30H gt M 19 Water M H30 M 45 Formic acid M HCOO Isolera Dalton Getting Started Guide Biotage 2015 General Information Consumables and Accessories Only genuine Biotage consumables and accessories must be used in the system To order consumables and accessories see contact information on the back of this document or visit our website www biotage com Accessories that may be necessary forthe Maintenance section in this document are listed below Part no Description 413460SP Solvent inlet tubing with inlet filters for Isolera Dalton Nanolink qty 3 414632SP Split flow interface SFI with tubing qty 1 413875SP External tubing kit for Isolera Dalton Nanolink qty 1 of each tube 413460SP and 413741SP see above is not included 413480SP External check valve for the direct injection port qty 2 413483SP Microfilter holder with filter qty 1 413484SP Microfilter qty 5 413487SP Needle port for direct injection qty 2 413710SP 250 ul gastight syringe qty 1 413711SP spraychip qty 1 413712SP vac chip qty 1 413714SP Maintenance kit for the active splitter qty 3 413715 Calibration kit for Isolera Dalton Mass Detector qty 1 413743SP Direct flow interface DFI qty 1 413890SP Tubes 20 x 150 mm for c
24. der of 1 pl min Incorporating an active splitter module between the flash purification system and the mass detector enables conversion to the correct flow for detection purposes and allows for mass analysis through direct injection of samples Isolera Dalton Software The Isolera Dalton software is designed to control Isolera Dalton Mass Detector and Isolera Dalton Nanolink The software can be installed on Isolera One and Isolera Four systems with an Isolera Spektra license Isolera One and Isolera Four with an Isolera Spektra License Isolera One and Isolera Four are flash purification systems that allow the user to set up control and monitor purifications Isolera Spektra is a software upgrade package that features a TLC to Step gradient calculator A All detection baseline correction 3D absorbance spectrum for the whole detector range and real time PDA scanning For more information please refer to Isolera Installation and Safety P N 411828 Isolera User Manual P N 411829 and Isolera Quick Guide P N 411830 Safety Before performing any procedures in this document please read and observe the safety requirements in the Isolera Installation and Safety document P N 411828 and Isolera User Manual P N 411829 Failure to follow those requirements may result in personal injury and or equipment damage To guarantee safe and effective operation it is absolutely
25. diameter of 20 mm to avoid damaging the vac chip Three are supplied with the mass detector 5 Slowly raise the test tube to allow the vac chip to slowly Slide down to the bottom of the tube 6 Pour enough HPLC grade water into the test tube to cover the vac chip 7 Place the test tube in a suitable rack in the ultrasonic bath and sonicate for 10 minutes Note Do not heat the ultrasonic bath 8 Remove the test tube from the bath and carefully pour out most of the liquid without removing the vac chip 9 Repeat steps 6 to 8 with HPLC grade acetonitrile 10 Repeat steps 6 to 8 with HPLC grade methanol 11 Gently tip the vac chip into a shallow petri dish or onto a lint free tissue 12 Carefully pick up the vac chip using a pair of flat plastic tweezers by pinching either side of the larger metal SHIM and gently blow dry the vac chip with compressed air or nitrogen Maintenance 13 Place the vac chip in the oven at 75 C for 30 minutes to completely dry it The vac chip should now be clean and ready for use If the vac chip looks visually degraded or you have any queries please contact Biotage 1 Point Support before using the vac chip Note If an oven is not available place the vac chip on a lint free tissue and leave it for a few hours to dry completely 14 Put the vac chip back into the mass detector by following the rest of the steps in the vac chip Replacement Wizard Replace the vac chip A va
26. e 46 18 565900 Toll Free 800 18 565710 Fax 46 18 591922 Order Tel 46 18 565710 Order Fax 46 18 565705 order biotage com Support Tel 46 18 56 59 11 Support Fax 46 18 56 57 11 Part Number 413457 E JAPAN Tel 81 3 5627 3123 Fax 81 3 5627 3121 jp_order biotage com jp 1 pointsupport biotage com 2015 Biotage All rights reserved No material may be reproduced or published without the written permission of Biotage Information in this document is subject to change without notice and does not represent any commitment from Biotage E amp OE A list of all trademarks owned by Biotage AB are available at www biotage com legal Other product and company names mentioned herein may be trademarks or registered trademarks and or service marks of their respective owners and are used only for explanation and to the owners benefit without intent to infringe CHINA Tel 86 21 2898 6655 Fax 86 21 2898 6153 cn_order biotage com cn 1 pointsupport biotage com To locate a distributor please visit our website at www biotage com Biotage
27. e DFI into the mass detector 7 Infuse at least 150 ul of the syringe solution through the spraychip at 10 ul min until it is completely saturated The solution will drip off the end of the spraychip 8 Remove the spraychip from the DFI 9 Gently blow dry the spraychip with compressed air or nitrogen 10 Leave the spraychip for a few hours to dry completely The spraychip should now be clean and ready for use If the spraychip looks visually degraded or you have any queries please contact Biotage 1 Point Support before using the spraychip 11 Putthe spraychip back into the mass detector by following the rest of the steps in the spraychip Replacement Wizard Note If an increased delay is observed when using the cleaned spraychip clean it again If the delay continues to be unacceptable the spraychip must be replaced Figure 19 The setup for cleaning the spraychip The syringe pump syringe and direct flow interface are included in the calibration kit Replace the spraychip The spraychip may become blocked or dirty over time If the Spray current displays a red value during a mass detector function test you may need to clean or replace the spraychip Required Powder free gloves and a spraychip P N 413711SP 1 Press Main Menu in the right hand panel 2 Press System The Select User dialog opens 3 Select your username and press OK 4 If your account is password protected the Password dialog open
28. ect at Startup Help Tea Enable or disable automatic connection of the mass detector at system startup Changing this setting will require a restart of the system Communication The system has to be restarted for the new configuration to take effect Signal Range 4000 mV 1 Press Main Menu and then Shut Down 2 When the system has shut down switch it off Extended Flush Volume 3 Switch on the system 10 ml Max Dispense Rate enera Off 18010 i Maintenance Reporting 12 Turn off Isolera Dalton Nanolink using the power switch located at the rear 13 Turn off the mass detector using the power switch located at the rear 14 Disconnect the mass detector and Isolera Dalton Nanolink from Isolera One Four as described below Disconnect Isolera Dalton Mass Detector and Isolera Dalton Nanolink Warning Handle chemical and liquid waste according to the Safety Data Sheets and local national guidelines on laboratory safety procedures 1 Shut down the system as described on page 5 2 Disconnect the mass detector Isolera Dalton Nanolink and Isolera One Four from the mains supply 3 Disconnect the tube connected between the Isolera flow cell and Isolera Dalton Nanolink from the flow cell s upper port A 4 Disconnect the tube connected between the fraction collector and the extension connector B from the extension connector B and connect it to the flow cell s upper port A See also the flow
29. ected solvent is present in the solvent reservoir 1 of the air flush volume is used and that the waste reservoir waste 1 has sufficient capacity for the air flush vi Couple the cartridge s inlet and outlet tubes together vii Press Start and wait for the system to finish the air flush Empty the internal tubing of the mass detector and Isolera Dalton Nanolink of liquid by pressing Start Flush at the Mass Detector tab Wait for the system to finish the flush If you want to use Isolera One Four without the mass detector disable the automatic connection of the mass detector at system startup i Press Main Menu in the right hand panel ii Press System The Select User dialog opens ili Select your user name and press OK iv If your account is password protected the Password dialog opens Enter your password and press OK v Select the Detector tab vi Select the Connect at Startup text box in the Mass Detector field and select No The Restart Required dialog opens vil Press OK Press Main Menu in the right hand panel Press Shut Down in main menu and then Yes to confirm The Mass Detector dialog opens Press Shut Down and then Yes to confirm This vents the mass detector to atmospheric pressure and then shuts it down When the message It is now Safe to turn off the system appears on the screen turn off Isolera One Four The power switch is located underneath the touch screen Main Menu Conn
30. ed through dialogs appearing on the screen According to instructions given by the technical support staff from Biotage Within limits set by the system s technical specification Failure to follow those instructions and operate within the limits set by the technical specification may result in personal injury and or equipment damage Isolera Dalton System comprises the following separate units solera Dalton Mass Detector Isolera Dalton Nanolink Isolera Dalton software Isolera One or Isolera Four with an Isolera Spektra license Isolera Dalton Mass Detector Isolera Dalton Mass Detector is a compact single quadrupole mass spectrometer built using micro electromechanical systems MEMS technology Isolera Dalton Mass Detector uses an electrospray ionization ESI source to produce ions which can then be identified by their mass to charge ratio m z Isolera Dalton Mass Detector allows you to analyze samples and automatically use the m z ratio s of the identified substance s for flash purification Isolera Dalton Nanolink Isolera Dalton Nanolink is an integration module intended for use together with Isolera Dalton Mass Detector and Isolera One or Isolera Four The flow rates of Isolera One Four are in Intended Use and Safety the order of 10 to 100 ml min These rates are too large for the microspray operation of Isolera Dalton Mass Detector where the required flow rates are in the or
31. em Care Guide document P N Ul320 Replace External Tubing Note All tube types dimensions and lengths are essential for the performance of the system Only replace tubes with the equivalent tubes supplied by Biotage 1 Shut down the system as described on page 5 2 Replace damaged tubing 3 Verify that tubes are assembled and inserted correctly see the Verify the System Setup section on page 9 Sonicate Solvent Inlet Filters The solvent inlet filter is installed on the end of each solvent inlet line on Isolera Dalton Nanolink P N 413460SP inlet lines and filters and Isolera One Four P N 412720SP filters These filters should be cleaned Sonicated or replaced every 1000 hours of operation or every 12 months whichever comes first Clean the Exterior Warning Always disconnect the equipment from the mains supply before cleaning the exterior surfaces to avoid the risk of electric shock 1 Shut down the system as described on page 5 2 Disconnect the power cords from the power outlets 3 Clean the exterior surfaces of the mass detector and Isolera Dalton Nanolink using a soft and clean cloth The cloth can be dry or lightly dampened with 10 aqueous isopropyl alcohol After cleaning wipe dry with a clean lint free cloth 4 To clean the touch screen and the exterior of Isolera One Four see the Maintenance section in the Isolera User Manual P N 411829 Maintenance of Isolera
32. en 3 When the analysis is completed copy the identified m z ratio s to the current method by pressing Save to Editor and Close in the last step of the wizard The selected spectrogram will be included in the archive report Figure 14 The sample to be analyzed should be injected into the DIRECT INJECT port in a slow steady flow when prompted by the Mass Analysis Wizard Run the Purification 1 Load the cartridge and collection rack s that you want to use 2 Ensure that a sufficient quantity of the correct solvent is present in each solvent reservoir and that the waste reservoirs have the sufficient capacity for the run 3 Press Run The Run Parameters dialog opens If you are using a system with four cartridge positions select the cartridge position to be used v 5 Select the rack position s to be used V Press Equilibrate gt The system starts the equilibration and switches to the Status tab where the progress can be monitored 7 When the equilibration is finished press Load Sample to enable sample injection The Load Sample dialog opens Prepare and Run a Purification 8 Inject your sample into the cartridge inlet Luer fitting using a syringe For ideal loading do not apply high manual pressure with the syringe Note The sample is the undiluted form of the mixture that you may have analyzed to set up the method Note See the Isolera User Manual P N 411829 for cartridge loading capa
33. ent If you also want to fill the liquid lines from the pump to the waste valve with the same solvent we recommend that you prime with at least 100 ml Select the Flowrate text box and enter the flow rate The maximum flow rate that can be used depends on the cartridge type mounted on the system if you selected the With Cartridge path in step 6 above the maximum fill rate s defined for the used solvent s in the Data Administration mode and the maximum dispense rate of the system 100 ml min when using the mass detector otherwise 200 ml min Enter the percentage of each solvent connected to the system that shall be used in the prime To start priming press Start Set Up the Method For more information you can at any time press Help to open the online help 1 2 Select the Method tab in the right hand panel To set up a new method press New or Wizard The later option opens the method wizard which will guide you step by step through the setup of a purification witha gradient including up to three steps using two solvents When done press Save to Editor in the wizard and proceed to step 7 To open and edit an existing method press Open and select the method in the dialog that opens Select the Gradient tab and create the desired gradient using the gradient table and or the gradient graph To show or hide the gradient table press the Table button W the gradient table is shown Note Alwa
34. l tubing or clean the exterior of the system See the shutdown procedure on page 5 Isolera Dalton Nanolink may be switched off when not in use but must be started before Isolera One Four is turned on Verify the System Setup Warning e Ensure that the power cords and any cables hoses and tubing connected to the system cannot come in contact with water or chemicals e If a leakage is detected immediately turn off the Isolera system disconnect the power cord from the power outlet and handle the leakage as described in the Leaks section on page 18 Isolera Dalton Mass Detector Verify that the mass detector is connected to a nitrogen gas supply with a pressure of 2 to 6 bar and a purity of 99 9 Only use clean stainless steel or PTFE tubing and fittings for the nitrogen gas line to avoid contamination Verify that the waste outlet tube at the front of the mass detector is inserted into a waste reservoir Due to the vacuum it is important that you never allow the waste outlet tube to become immersed in the waste liquid Isolera Dalton Nanolink Verify that Isolera Dalton Nanolink is placed on the tray on top of the mass detector System Setup Verify that the waste outlet tube on the right hand side is inserted into a waste reservoir Verify that the drain tube connected to the tray is inserted into a separate waste reservoir or placed on the Isolera leak tray if using Biotage Leak
35. leaning the vac chip gty 3 General Information Manufacturers Microsaic Systems plc for Biotage Sweden AB Isolera Dalton Mass Detector PartnerTech Atvidaberg AB for Biotage Sweden AB Isolera One Isolera Four and Isolera Dalton Nanolink Contact Us Biotage Sweden AB Box 8 SE 751 03 Uppsala SWEDEN Visiting address Vimpelgatan 5 Phone 46 18 56 59 00 Fax 46 18 59 19 22 E mail info biotage com Website www biotage com Please contact your local Biotage representative See contact information on the back of this document or visit our website www biotage com 21 Your Complete Partner for Effective Chemistry Biotage is a worldwide supplier of instruments and accessories designed to facilitate the work of laboratory chemists With our deep knowledge ofthe industry academic contacts and in house R amp D teams we can deliver the best solutions to vour challenges We take great pride in our flexibility and ability to meet our customer s individual needs With strong foundations in both analytical and organic chemistry we can offer the widest range of solutions available on the market EUROPE NORTH amp LATIN AMERICA Main Office 1 704 654 4900 Toll Free 1 800 446 4752 Fax 1 704 654 4917 Order Tel 1 704 654 4900 Order Fax 1 434 296 8217 ordermailbox biotage com Support Tel 1 800 446 4752 Outside US 1 704 654 4900 eu 1 pointsupport biotage com us 1 pointsupport biotage com Main Offic
36. matter e g molecular sieve is present in the reservoirs If necessary filter the solvents Fill the four reservoirs with the solvents to be used and connect them to the inlets on the right hand side of Isolera One Four Prepare and Run a Purification Assign Solvents to the Solvent Inlets on Isolera One or Isolera Four When a purification is run the software references the solvent assignments to determine which solvent inlets that are connected to the solvents used in the method 1 Select the Setup tab in the right hand panel Select the Instrument Solvents tab Select the solvent that the reservoir connected to the selected solvent inlet contains The software comes with a preconfigured list of solvents and their parameters 2 3 Press one ofthe Solvent text boxes 4 To add a solvent press New To edit a user defined solvent select the solvent and press Edit 5 If solvent monitoring is enabled i Select the Capacity text box and enter the capacity of the solvent reservoir ii Select the Current text box and enter the current solvent level of the reservoir 6 Repeat step 3 through 5 for all solvent inlets All solvent inlets must be primed with solvent Note If monitoring of solvent and or waste levels is enabled you have to enter the capacities and current fluid levels for the solvent and waste reservoirs connected to Isolera One Four each time you empty a waste reservoir or replenish a solvent
37. n the right hand panel Ensure that the solvents are assigned accurately to the solvent inlets at the Instrument Solvents tab Select the Prime tab If you are using a system with four cartridge positions select the Channel text box and select the cartridge position and waste reservoir to be used 6 Select the Path text box and select the prime path To only prime the solvent inlet s select Bypass To also prime the cartridge channel select one of the channel options 7 Ifyou selected the Without Cartridge path couple the cartridge tubes together 8 If you selected the With Cartridge path select the Cartridge Instrument Solvents Parameters Path Skip Volume Warm Up Flowrate gt Without Cartridge Resume Solvent 2 Ethyl acetate Type text box and select the cartridge type mounted on the system Air Flush Mass Detector Main er Path Path Select the prime path To only prime the used Bypass solvent inlet s select Bypass To also prime the cartridge channel select a channel option If selecting Without Cartridge couple the 0 6 bar cartridge tubes together Mass Detector Help Method Solvent 1 n Hexane Prime the solvent inlets on Isolera One or Isolera Four at the Prime tab 9 10 11 12 Select the Volume text box and enterthe total prime volume If you have filled a solvent inlet with a new solvent we recommend that you prime with at least 40 ml of that solv
38. necessary to follow all of the safety precautions and instructions in the Isolera user documentation supplied by Biotage Translated versions of the Safety chapter in the Isolera Installation and Safety document are available in the Isolera Safety Translations document P N 412861 Download Isolera User Documentation To download the user documentation from the system connect a USB memory device to the USB port located underneath the touch screen press Help and then press Export User Documentation You can download the latest versions of the documents at www biotage com If you have problems downloading please contact your local Biotage representative System Overview System Overview Isolera Dalton Nanolink Isolera One or Four Isolera Isolera Dalton Mass Detector Isolera Dalton Software Dalton System Basic Functionality A chemical sample containing one or more components and dissolved in suitable solvent s can be injected into the system to identify characteristic m z ratio s for the substance s of interest The detected m z ratio s can be used for identification and collection of specific components during a chromatography run The purposes of the units in the system are Isolera One Four controls all units through the touch screen software and performs the flash chromatography Isolera Dalton Nanolink is used as an active spli
39. o refer to the Isolera Dalton System Care Guide document P N Ul320 Mass Detector Function Test Ifthe system is malfunctioning we recommend that you perform a mass detector function test as described on page 10 See below some actions for flow pressure and signal errors Flow Pressure and Signal Errors If there is no spray current during a method run or mass detector function test there could be an issue with the flow to the mass detector or a blockage in the spraychip This may also pop up as an error dialog with the text LOW SPRAY CURRENT or FAULT Verify that there is a flow to your mass detector by observing droplets from the waste outlet tube during a mass detector function test signal or baseline If droplets are observed but there is still no spray current replace the spraychip as described on page 16 If the mass signal during a method run or a mass detector function test appears very unstable it may indicate airin the tubing Flush the mass detector and Isolera Dalton Nanolink tubing see page 15 or prime the makeup solvent inlets see page 10 If a low mass Signal is observed during a mass detector function test signal this may indicate a blocked or partially blocked vac chip Clean or replace the vac chip as described on page 16 The makeup flow pressure normally operates between 2 0 and 6 5 bar If the makeup flow pressure is Lower than 2 bar when the makeup pump is running this
40. r direct injection is leaking when the Isolera pump is running the check valve P N 413480SP may need to be cleaned or replaced See Leakage at the Direct Injection Port on page 18 If leakage is detected on the Isolera Dalton Nanolink tray or via the drain tube connected to the tray then the leak is likely located inside Isolera Dalton Nanolink Please contact Biotage 1 Point Support If the splitter valve leaks between the stator and stator ring see image on page 18 or from a port the rotor seal and stator face assembly may have been damaged by abrasive particles in the sample and or the makeup solvents Replace the rotor seal and stator face assembly using the maintenance kit supplied by Biotage P N 413714SP Instructions are provided in the kit When done reset the counter for active splitter switches as described on page 18 If the leakage is detected on Isolera One Four see the Leaks section in the Isolera User Manual P N 411829 Troubleshooting of Isolera One and Isolera Four See the Troubleshooting section in the Isolera User Manual P N 411829 20 Hints and Tips Hints and Tips Some Commonly Quoted Volatile Additives and Buffers Recommended Volatile Additive or Buffer Empirical Formula pKa Formic acid HCOOH 3 6 Ammonium hydroxide NH4OH 9 2 Commonly Observed Adduct lons From Buffer Additives at 50 V Mass of Adduct Ion Source of Adduct Ion Formula of Addu
41. re that system is not processing before removing the needle port or check valve Figure 20 The direct injection port assembly needle port A adapter B and check valve C Flush the Isolera Dalton Nanolink Tubing Never leave Isolera Dalton Nanolink with DCM Flush the mass detector and Isolera Dalton Nanolink tubing with neutral solvent makeup solvent and methanol or similar Isolera solvent as described in Flush the Mass Detector Tubing on page 15 Replace the Rotor Seal and Stator Face Assembly in the Active Splitter Ifthe splitter valve leaks between the stator and Body Stator ring or from a port Shaft Assembly the rotor seal and stator face assembly may have Co Pato Sea been damaged by abrasive a oe particles in the sample and or the makeup solvents and cs Stra need to be replaced The rotor seal and stator face assembly also have to be replaced when the active splitter has switched more than 1 million times The user will be alerted at system startup Stator Screws Required Maintenance kit for the active splitter P N 413714SP 1 Replace the rotor seal and stator face assembly using the maintenance kit supplied by Biotage P N 413714SP Instructions are provided in the kit 2 Reset the counter for the active splitter switches i Press Main Menu in the right hand panel ii Press System The Select User dialog opens ili Select your user name and press OK iv If yo
42. s Enter your password and press OK Select the Maintenance tab VI 6 Press Replace spraychip in the Mass Detector field and follow the instructions appearing on the screen Isolera Dalton Getting Started Guide Biotage 2015 Clean the vac chip Avac chip blockage may be indicated by 1 a low pressure reading of the ion guide IG vacuum or 2 a low mass detector signal when running a mass detector function test signal Clean or replace the vac chip Warning e Handle chemical and liquid waste according to the Safety Data Sheets and local national guidelines on laboratory safety procedures e Appropriate safety precautions must be taken when using a ultra sonic bath see the manufacturer s instructions Required A clean test tube with an inner diameter of 20 mm supplied with the mass detector P N 413890SP a pair of flat tweezers supplied with the mass detector an ultra sonic bath a petri dish deionized water methanol and acetonitrile 1 Start the vac chip Replacement Wizard see Replace the Spraychip above 2 Follow the instructions appearing on the screen When the vac chip has been removed clean it as described in steps 3 to 13 below 3 Prepare a small ultrasonic bath in a fume hood Fill the bath with room temperature water 4 Hold the test tube horizontally and carefully place the vac chip just inside the brim of the tube Note Always use a clean test tube with an inner
43. s required for analysis and it aligns the ions from the spray chip into the vacuum system through the vac chip lon optics The ions generated from the spraychip enter the vac chip and are focused into the ionchip using the ion optics Vacuum system This consists of a vacuum chamber coupled to two turbo molecular pumps which are supported by a small diaphragm pump All pumps are integrated within the mass detector jonchip The ion chip is a quadrupole that filters the ions according to their mass to charge m z ratios and directs them into the detection system Door with a safety interlock system to protect users from high voltages see Safety Interlock below Safety Interlock The mass detector has a safety interlock system to protect users from high voltages This system is operated by the door in the front cover Figure 2 To protect the users high voltages are disabled when the mass detector door is open When the door is shut the safety interlock is activated high voltages can be applied and the user is able to run the mass detector When the door is open the safety interlock is deactivated and high voltages are disabled A click will verify the position The door will remain fixed in this position until pulled off its catch With the door open and the safety interlock deactivated replacement of the spraychip and vac chip see the Maintenance section on page 15 can be carried out with the m
44. s System The Select User dialog opens Select your user name and press OK mB W N If your account is password protected the Password dialog opens Enter your password and press OK P Select the Maintenance tab 7 Press Calibrate in the Mass Detector field and follow the instructions appearing on the screen Clean the spraychip The spraychip may become blocked or dirty over time If the spray current displays a red value during a mass detector function test you may need to clean or replace the spraychip Warning Handle chemical and liquid waste according to the Safety Data Sheets and local national guidelines on laboratory safety procedures Required HPLC grade methanol and water a lint free tissue and the calibration kit supplied with the mass detector P N 413715 1 Start the spraychip Replacement Wizard see Clean the Spraychip above 2 Follow the instructions appearing on the screen When the spraychip has been removed clean it as described in steps 3 to 10 below 3 Fill the syringe included in the calibration kit with a 1 1 mixture of HPLC grade methanol and water with no additives 4 Setup the syringe pump syringe and direct flow interface included in the calibration kit as shown in Figure 19 below 5 Screw the spraychip to be cleaned into the direct flow interface DFI and tighten the grub screw 6 Place the DFI on a lint free tissue on a flat surface Note Do not put th
45. schemes on page 7 5 Disconnect the two communication cables see scheme on page 8 6 Disconnect the mass detector from the nitrogen gas supply 7 Disconnect the filter unit C from Isolera Dalton Nanolink by loosening the peek nut D and pulling the filter unit out Isolera Dalton Getting Started Guide Biotage 2015 Isolera Dalton Nanolink Fraction collector Isolera One or Isolera Four Isolera Dalton Mass Detector Waste Installation Isolera Dalton Nanolink Fraction collector Isolera One or Isolera Four Isolera Dalton Mass Detector Figure 8 Flow schemes illustrating when Isolera Dalton Mass Detector and Isolera Dalton Nanolink are connected left and disconnected right 8 Empty the waste reservoirs connected to 1 the waste outlet tube on the right hand side of Isolera Dalton Nanolink 2 the waste outlet tube at the front of the mass detector and 3 the drain tube on the tray 9 Ifyou want to move the system proceed to the Move the System section below Warning Keep your hands out of range of the collection arm while the homing routine runs in step 10 below 10 If you want to use Isolera One Four without the mass detector connect it to the mains supply an turn it on The collection arm moves through its homing routine and the system boots to the system s main menu Move the System Warning e Isolera Dalton Mass Detector weighs
46. ted onto the tube ends as described in the instructions supplied with the ferrules Use caution when finger tightening fittings to prevent stripped threads or crushed ferrules jui Figure 11 Ferrule with the tapered portion facing toward the nut Prepare and Run a Purification Prepare and Run a Purification Start the System Warning Keep your hands out of range of the collection arm while the homing routine runs in step 3 below 1 Turn on Isolera Dalton Nanolink using the power switch located atthe rear 2 Ifthe mass detector is not already turned on turn it on using the power switch located at the rear and then the power switch at the front 3 Wait at least 2 minutes and then turn on Isolera One Four using the power switch located underneath the touch screen The mass detector should be allowed to pump down adequate vacuum and to stabilize when turned on The complete process takes 30 minutes Prepare Isolera Dalton Mass Detector and Isolera Dalton Nanolink for a Run Load the Makeup Solvents Note Always use methanol of LC MS grade and purified water Note Ensure that no foreign matter e g molecular sieve is present in the reservoirs If necessary filter the solvents Fill the three 1 liter bottles with the solvents to be used and connect them to the correct inlets on the right hand side of Isolera Dalton Nanolink Neutral methanol water 9 1 0 5 formic acid in methanol w
47. to detect leakage 11 Carefully lift Isolera Dalton Nanolink and place it on the tray on top of the mass detector 12 Insert the waste outlet tube on the right hand side of Isolera Dalton Nanolink into a waste reservoir 13 Insert the waste outlet tube at the front of the mass detector into a waste reservoir Due to the vacuum it is important that you never allow the waste outlet tube to become immersed in the waste liquid 14 Proceed to step 5 in the Reconnect Isolera Dalton Mass Detector and Isolera Dalton Nanolink section on page 8 Installation Isolera One or Isolera Four M LE Isolera Dalton Mass Detector Isolera Dalton Nanolink O amp CA Figure 9 Scheme for connecting and disconnecting the communication cables a USB cable between Isolera One Four and Isolera Dalton Nanolink and an Ethernet cable between Isolera One Four and the mass detector Reconnect Isolera Dalton Mass Detector and Isolera Dalton Nanolink 1 Ifreconnecting after a move of the system proceed to step 5 2 Empty the tube connected between the fraction collector and the flow cell using the air flush function see step 5 in the Shut Down the System Not for Daily Operation section on page 5 3 Enable the automatic connection of the mass detector at system startup i Press Main Menu in the right hand panel ii Press System The Select User dialog opens iii Select your user name and press
48. tter for sampling a small portion from the larger flash chromatography flow into the mass detector It also enables mass analysis via direct injection of samples Isolera Dalton Mass Detector performs the detection and supplies information to the software when to collect and fractionate the sample Isolera Dalton System can also be programmed to perform the following functions Generate user defined elution gradients Store and implement a large number of independent chromatographic methods Control and collect fractions based on UV visible light absorbance Produce detailed printable and searchable reports on mass analysis and purification Setup Example LI PUPILI Figure 1 Left top Isolera Dalton Nanolink and tray Left bottom Isolera Dalton Mass Detector Right Isolera Four with an Isolera Spektra license System Flow Scheme The left flow scheme on page 7 illustrates the flow when Isolera Dalton Mass Detector and Isolera Dalton Nanolink are connected to Isolera One Four Isolera Dalton Getting Started Guide Biotage 2015 Isolera Dalton Mass Detector Basic Components spraychip The spraychipis a factory calibrated disposable nanospray interface A chemical sample dissolved in suitable solvents is introduced into the spraychip from Isolera Dalton Nanolink vac chip The vac chip is a vacuum interface It allows the mass detector to achieve the operating pressure
49. ur account is password protected the Password dialog opens Enter your password and press OK v Select the Maintenance tab vi Press Reset Active Splitter Switches in the Mass Detector field Replace the Microfilter If high back pressure is detected in the makeup pump lines and the High Makeup Flow Pressure dialog appears the microfilter is probably partially clogged and needs to be replaced Note The filter unit contains methanol 1 Ensure that the system is not processing 2 Disconnect the filter unit A from Isolera Dalton Nanolink by loosening the peek nut B and then pulling the filter unit out 3 Carefully open the filter unit and remove the microfilter C 4 Insert a new microfilter and reassemble the filter unit turning it clockwise Ensure that the peek tube D is sticking out of the ferrule a few millimeters 5 Reattach the filter unit to Isolera Dalton Nanolink 6 Perform amass detector function test for approximately 1 minute see instructions on page 10 The pressure should remain at a low level throughout the test preferably between 2 and 5 bar If the pressure is still high the stator face assembly may need to be replaced see instructions above Maintenance of Isolera One and Isolera Four See the Maintenance section in the Isolera User Manual P N 411829 Isolera Dalton Getting Started Guide Biotage 2015 Troubleshooting Please als
50. ys add an equilibration step of at least 2 CV to avoid clogging of the mass detector and Isolera Dalton Nanolink Select the Parameters tab and select the solvents cartridge type and rack type to be used Select the Collection tab and specify the collection and fractionation settings to be used To identify the m z ratio s for the substance s of interest see the Analyze the Sample section on page 13 If you want to save the method to be able to reuse it in the future press Save As Note You do not have to save a method to run it Proceed to the Run the Purification section on page 13 Isolera Dalton Getting Started Guide Biotage 2015 Analyze the Sample A chemical sample containing one or more components and dissolved in suitable solvent s can be injected into the system to identify the m z ratio s for the substance s of interest Note Always use a clear and filtered 0 5 um or less pore size sample for analysis to avoid clogging Required The 250 ul syringe supplied with Isolera Dalton Nanolink P N 413710 sample and methanol 1 Prepare the sample i Make a diluted solution of your sample approximately 1mg mlin methanol or another solvent ii Filter 0 5 um or less pore size your sample carefully to remove any particles that may clog the system 2 Press Mass Analysis at the Method tab This opens the Mass Analysis Wizard Follow the instructions appearing on the scre

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