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1. P N PAL NdlSeal Teflon tube with stainless steel ferrule for Gauge 22 needles standard Seal for valve bore 0 25 and 0 40 mm Teflon transparent P N PAL NdlSealP Teflon Tube with PEEK ferrule for Gauge 22 needles Seal for PEAK Valve bore 0 40 mm Teflon transparent P N PAL NdlSeal 19 Teflon Tube with stainless steel ferrule for Gauge 19 needles Seal for Prep Valve Bore 0 75 mm Teflon blue color note For the PEAK Valve it is crucial that all ferrules used for any connection are made out of PEEK Stainless steel ferrules are too hard One does risk to crack the PEAK valve stator using a steel ferrule note Jo ensure reproducible sample injection and minimize carryover it is critical that e The valve needle guide and the valve needle seal are installed properly e The valve needle seal is changed every 1500 2000 penetrations e The needle penetration depth is set accurately see chapter 9 3 Injection Valve Needle Penetration 66 note l note l IFC PAL User Manual 9 3 Injection Valve Needle Penetration Before performing the following steps make sure the Object Position X Y Z for LC Vivi LC Viv2 are properly defined and a syringe adapter including a syringe is inserted in the Injection Unit see chapter 7 2 and 8 3 Complete the following steps to define the Valve Needle Penetration Depth In the Object Class Injectors choose the Object LC VIv1 The following screen is displayed Menu
2. IFC PAL User Manual How to Use this Manual The manual is divided into three major sections IFC PAL Operating Instructions Section A IFC PAL Description and Installation Section B Appendices The IFC PAL Operating instructions in Section A are intended for infrequent PAL users or new users that are experienced in using automated systems to perform existing analytical methods The IFC PAL must be installed and set up properly before the Operating Instructions in Section A can be used Users who are installing a IFC PAL system IFC PAL accessories or who need to make adjustments to an installed system should consult IFC PAL Description and Installation in Section B The Appendices provide useful information such as the Software Flow Chart Definition of Terms or the IFC PAL Accessories guide IFC PAL User Manual A IFCPAL Operating Instructions The IFC PAL has to operated bv a dedicated software example IFC PAL Software provided by CTC Analytics The IFC PAL can also be integrated in other manufacturer software The IFC PAL can not be operated as a standalone unit All functions shown and explained in this Chapter A IFC Operating Instructions have to be considered as an instruction to install trouble shoot or how to change a syringe as an example The general functions of the Control Terminal are exactly the same as described for other PAL Systems If the customer wishes to use the Injector side of the
3. IFC PAL User Manual Printing Historv Edition 1 October 2003 Software Version 2 5 0 The PAL Svstem mav be operated with another level of firmware Details of the current level are given with the leaflet Firmware Overview which is placed in the front of this binder CTC Analytics AG reserves the right to make improvements and or changes to the product described at any time without notice CTC Analytics AG makes no warranty of any kind with regards to this product including but not limited to the implied warranties or merchantability and suitability for a particular purpose In no case shall CTC Analytics AG be liable for any coincidence ore consequential damages in connection with or arising from the use of this document 2003 CTC Analytics AG All rights reserved Neither this publication nor any part of this publication may be copied photocopied reproduced translated or reduced to any electronic medium or machine readable form without the prior written permission of CTC Analytics AG except as allowed under the copyright laws CTC Analytics AG acknowledges all trade names and trademarks used as the property of their respective owners Declaration of Conformitv General Considerations IFC PAL User Manual Safety Information See Declaration of Conformity sheet enclosed with the instrument A Changes or modifications to this unit not expressly approved by the party responsible for compliance could void the u
4. awy Sunpog anos JEN IMA iuad IPN 7 uonsod JPUB4 3paaN A UOIISOg 7 U0150d x uonsod A UOIJISOd NEM K LOIJIEOA par AME ZUSEM Ipuag APAN iauad 3paaN 7 UONSOd 7 UOIyISOd A UOLSOg A UOIMSOd x UOIIBOg X UDIMISOA INA DI IUSEM SUU PIA 7 PSJJO APSHO X BSJO IU BH EIA adij Aij Jap OH Aba Ruz ZPSHO APSO B PHO 1Y813H PIA addy 4 L PPH fel Lgu ZPYO ASHO XK PSO 14819 JEA 30A Api Jap PH Ae R ZPYO APSO X PSJO 14819 JEHA adi JI HPPH Aes ZLIMHOLW PSO APSHO X PSHO 1819 FEIA 2A AIl Jap PH Aes SOM L0MA y uosinay qied aopay Jed 5399y 7 uonsod A UOQBOd K UOQBOd UPIHL Yl D10pay Jed S304 7 UOQSOJ A U0N60d X UOQEO4 DES ied 2JO AN Ed 5929 7 WONSOd A UOQEOJ X UDIBOg pers 88 E External Connectors Connector SERI Pin Signal Name DCD RXD TXD DTR GND DSR RTS CTS RI WO CON DM OT PI WIN Connector SER2 SER3 Pin Signal Name GND RXD TXD RTS CTS 5V reserved reserved CON D OB WN IFC PAL User Manual 89 IFC PAL User Manual Connector INTERFACE 1 8 1 39999999 O gagggaa f O 15 g Pin Signal Name 1 Pwr Out1 2 Pwr Out2 3 SW Out1 NO 4 SW Out1 COM 5 SW Out2 NO 6 Opto Ini 7 TTL In1 8 GND 9 Pwr Outl 10 Pwr Out2 11 TIL In2 12 SW Out2 COM 13 TTL In3 14 Opto In1 15 5V Connector INTERFACE 2
5. ji Info Update Backup Setup Start Pal e Figure 41 PAL Loader menu screen 4 Click the Backup button A dialog box entitled Backup Target Memory will be displayed The path storage location and file name to be assigned to the new backup will be shown A customized path and or filename may be entered Backup arget Memory Filename CAPR OGRAMMENPALNLOADERNBACKUPNBE 9810825 Browse Backup Log Backup Figure 42 PAL Loader Backup Target Memory 69 note l IFC PAL User Manual Click the Backup button Backup will proceed and information on the backed up components will be displayed in the Backup Log window The process will take several minutes The message Backup of Target Memory succeeded indicates a successful backup Click the Close button to exit the Backup dialog box Click the Start PAL button to terminate control by the Loader program On the Keypad terminal the Job Queue screen is displayed Disconnect the RS 232 cable from the PAL 11 2 Reloading a Backup This operation can potentially overwrite existing parameter settings Methods created by the user will be overwritten The firmware file to be loaded must reside on the PC hard drive The file cannot be loaded from a floppy drive A full update including parameter settings will not fit on a single floppy diskette in the PAL Loader format It must be transferred to the PC hard drive in compress
6. 1 0 RSD of peak area Carryover Typically lt 0 1 Sample Capacity Collector Side 14 standard Trays to hold reagent tubes with various volumes Tube OD 25 mm holding 55 ml 21 Tubes per Trayholder total 294 tubes Tube OD 20 mm holding 35 ml 39 Tubes per Trayholder total 504 tubes Tube OD 18 mm holding 27 ml 50 Tubes per Travholder total 700 tubes Tube OD 16 mm holding 16 ml 50 Tubes per Travholder total 700 tubes Tube OD 13 mm holding 09 ml 78 Tubes per Trayholder total 1092 tubes Volume given for tubes with 1500 mm height Trayholders for tubes with 100 mm height are available Collector Syringe Volume 2 20 80 200 and 800 ul syringes available Dead Volume for changes Collect Waste in ul range Injection cycle time Typically 1 to 3 minutes depending on plunger speeds injection volume and wash cycles 29 IFC PAL User Manual 5 3 Electrical Specifications Parameter Protection Class Class Over Voltage Category Category ll Pollution Degree 2 Moisture Protection Normal IPXO a Protection Class Protection class describes the insulating scheme used in the instrument to protect the user from electrical shock Class identifies a single level of insulation between live parts wires and exposed conductive parts metal panels in which the exposed conductive parts are connected to a grounding system In turn this grounding system is connected to the third pin ground pin on the electr
7. 70 1 73 15 74 Lo 6 80 dl Appendices A Definition of Terms B Conventionsof Naming C HTS PAL Injection Cycle D Software Flow Chart E External Connectors IFC PAL User Manual 58 58 59 60 65 65 List of Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Figure 11 Figure 12 Figure 13 Figure 14 Figure 15 Figure 16 Figure 17 Figure 18 Figure 19 Figure 20 Figure 21 Figure 22 Figure 23 Figure 24 Figure 25 Figure 26 Figure 27 Figure 28 Figure 29 Figure 30 Figure 31 Figure 32 Figure 33 Figure 34 Figure 35 Figure 36 PAL Control Terminal and Conventions Accessing a Method Screen Example Job Queue Screen IFG PAL Major System Components for Analytical Version IFG PAL Major System Components for Preparative Version Attachment of Mounting Claws Attaching the PAL Injection Unit Connecting the Injection Unit Flat Cable Inserting the Injection Unit Mounting Torx Screws IFC PAL with Injection Unit and Standalone Supports Installing Keypad Terminal Installing the Injection Valve Drive Installing the Fast Wash Station Fast Wash Station Assembly Electrical Connection Fast Wash Station Installing a Microplate Stack Installing a Trayholder IFC PAL Support Leg Transport Lock IFC PAL Straining of Support legs IFC PAL Assembling Tray Pan and X Y Axis IFC Assembly Front View IFC PAL Assembling as an Example Configurati
8. Setup Injector LC Vivl Position Y 2 6mm Objects Position Z 86 Omm Needle Penetr 20 0mm Valve DC6 1 C 1998 08 31 11 20 25 Check Clear Movto Home Pos Pos Zero Figure 40 Menu Screen Valve Needle Penetration Depth Press the FI button Check Pos The Injection Unit moves to the previous defined LC Vlv1 position Highlight the ttem Needle Penetr with the cursor bars and press ENTER Slowly rotate the outer knob to adjust the Needle Penetration Depth The syringe moves down stepwise into the Injection port When the syringe needle tip enters the valve needle guide slow down the Z movement again Always observe the syringe needle during this operation step Move single step wise down until you notice a click sound inside the Injection Unit STOP immediately the Z down movement Rotate the outer knob two steps in the opposite direction and press ENTER to save the Needle Penetration Depth value Press F3 Movto Zero Verify the defined Needle Penetration Depth value by repeating Step 2 and 3 After all positions have been set and the Valve Needle Penetration has been adjusted perform a backup of the existing configuration see Chapter 11 PAL Loader Program 6 Menu IFC PAL User Manual 10 Interfacing the IFC PAL to Other Devices 10 1 Synchronization and Output Signals Synchronization Signals Sync Signals are inputs that tell the HTS PAL when to wait or proceed with a sample processin
9. The value may be changed for different types of syringes Ze IFC PAL User Manual 4 2 Tray After selecting the particular Tray to be accessed the following Functions are available Function Key Description F3 Movto nnn This function serves as a quick check to determine if the XYZ coordinates are defined correctly for the selected Tray To use this utility the selected Tray including the sample vials or Microplate must be present After pressing Movto 001 the Injection Unit moves to sample position no 1 This procedure can be repeated for the last sample position in the first row and the last sample position in the last row F4 HOME The Injection Unit moves to its HOME position and the Job Queue Menu is displayed The following Tray Parameters may be changed by selecting the particular item Item Description Needle Penetr Needle penetration depth into the sample vial The stored default values for each Sample Tray Type are approx 2mm above the sample vial Microplate bottom The needle penetration depth for the selected Tray may be changed by entering the desired value Tray Type The Tray Type which is selected for the Tray is shown If the Tray enables use of different Tray Types it can be changed here Alternate use of Microtiter or Deepwell plates in a Stack 4 3 Injector After selecting the particular Injector to be accessed the following Functions are available Function Key Description F1 Rinse Inj
10. replace and or clean the Syringe Press the Menu key to see the available options for changing F1 Change Syringe and cleaning F2 Clean Syringe To completely remove air bubbles the Syringe should be primed manually see chapter 8 2 page 32 Syringe priming Close all Stack drawers 20 1 3 2 3 3 IFC PAL User Manual If only one Job will be processed select that Job with the scroll knob Press Start key In the dialog box Select Job s to Process select one of the following options All Entire Job Queue starting from the top Selected Job selected with the cursor bars Resume Continue with the next Job after the aborted one Aborting a Job Queue Press STOP Select one of the available options Continue Sample Job or Job Queue Select Continue to resume processing with the current sample Select Sample to abort processing of the current sample Processing will resume with the next sample Select Job to abort processing of all samples in the current Job Processing will resume with the next Job The aborted Job is marked with an X Select Job Queue to abort processing of all Jobs The JOB QUEUE screen will be displayed The aborted Job is marked with an X Restarting an Aborted Job Queue Press the START key Select the option Resume The job after the last one marked as aborted will be started 21 note l 4 1 IFC PAL User Manual Utilitv Functions Utility functi
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12. 1 To copy a Method complete the following sequence Menu Methods Method name Copy Method 2 You will be prompted to enter a name for the new Method Use the scroll knob and the left right arrow function keys F2 and F3 to select among alphanumeric characters and spaces Press the ENTER function key F4 to accept the name 1 To create a new Method complete the following steps Menu Methods Select the insertion point Insrt Method 2 Assign and enter a new Method name as above After a copy of the Method has been created the Method parameters will be displayed and can be edited The Cycle and Syringe entries cannot be changed 3 If the Method is new i e added select and enter a Cycle that is appropriate for the application 4 Select the specific Syringe to be used by the Method Once a Method has been created and saved the Cycle and Syringe can not be changed To use a different Cycle or Syringe a new Method must be created 5 Assign Parameter values according to the application requirements Consult Appendix D HTS PAL LC Inj Cycle Parameter for details of the specific items The IFC can be used to Inject an analytical sample no fraction collector mode Therefore the HTS PAL Cycle has to be used IFC PAL User Manual 2 2 Edit View Methods Method parameters excluding Cycle and Syringe can be viewed and changed from the Method menu as follows Menu Methods Method name Enter NO Scroll to and select
13. 13 1 O 1233999999999 O 999999999999 25 14 Pin Signal Name 1 TIL InI 2 TIL In2 3 TIL In3 4 TIL Outi 5 TTL Out2 6 TTL Out3 7 Opto In1 8 Opto In2 9 SW Outi NO 10 SW Out2 NO 11 Pwr Out1 12 Pwr Out2 13 45V 14 19 GND 20 Opto In1 21 Opto In2 22 SW Outi COM 75 SW Out2 COM 24 Pwr Outl 25 Pwr Out2 90 Pin 1 53 2 4 5 7 6 8 10 16 18 11 12 13 14 15 17 19 20 Signal Name Motor Al Motor A2 Motor B1 Motor B2 GND Temp Temp Sens 5V Heater 36V Connector WASHSTATION Control Board l Pin 14 2 2 1 Signal Name Pwr Out1 Pwr Outl Pwr Out2 Pwr Out2 IFC PAL User Manual 91
14. Device Input Voltage 24 VDC Input Current Power Supply for PAL IFC Box Interface Box for Fraction Collector A D converter Optional Device Input Line Voltage Grounded AC 100 to 250 V 50 60H2 o O Input Line Frequency 50 60 Hz Input Power 0 7 0 35 A Output Voltage 5 VDC 15 VDC Output Current 1 0 A 0 4 A 0 4 A 32 IFC PAL User Manual 5 4 Physical Specifications IFC PAL Systems Analytical Version S rr Width qa IFC PAL Systems Preparative Version ooo Width 1428 mm 56 2 in ind Control Terminal on both sides 5 5 Operating and Environmental Requirements Bench Space At least 16 cm 6 in at the rear space for fluid waste container below the instrument and solvent containers next to the instrument Access to power switch es and power cord s Clean level and smooth surface Solid bench plate Negligible Negligible 99 note l note l IFC PAL User Manual 6 Installation 6 1 IFC PAL System Analytical Version 6 1 1 Unpacking the Components A IFC PAL System is shipped at least in two boxes One box contains the X Y Crossrail assembly the injection unit the keypad terminal standalone supports connecting cables power supply syringe kit the injection valve fast wash station assembly safety guard and miscellaneous parts The other box will typically contain Microplate Stacks and or Trayholders 1 Open the large box containing the X Y Crossrail First remove the In
15. IFC PAL Used for Analytical Flow Rate Range Typically 1 ml min or less Figure 4 IFC PAL Major System Components for Analytical Version The IFC PAL configuration can include a Microplate Stack Peltier cooled or not cooled a 6 port LC Injection Valve and a Fast Wash Station In addition a second valve drive two additional Microplate Stacks or Vial Tray Holders can be added 26 IFC PAL User Manual 5 1 1 Specifications for IFC PAL Analytical Version General Specifications Sample capacity 98 x 2ml vials per Tray 200 x Iml vials per Tray 32 x 10ml 20ml vials per Tray 6 Deepwell or Standard Microtiterplates in a 3 drawer Stack 12 Standard Microtiterplates in a 6 drawer Stack up to 4 Stacks Injector and Collector side may be configured max 24 plates for each side Thermostatted Sample Tray Optional 4 C 70 C Injection volume range 5 10 25 100 250 500 1000 2500 and 5000 ul syringes are available Down to 0 5ul with solvent sandwich injection Down to 0 5ul with optional 4 port internal loop configuration Up to 5000ul with optional larger loop and syringe Replicate injections 1 99 from one vial Wash Station 2 different wash solvents Precision Typically lt 0 5 RSD of peak area from 10 ul 100 ul Typically lt 1 0 RSD of peak area from lt 10 ul Carryover Typically lt 0 1 See specific Specification Data Sheet Collector Syringe Volume 2 20 80 200 and 800 ul syringes available Dea
16. In case of any failure contact a representative of CTC Analytics 80 IFC PAL User Manual 14 2 Maintaining the Sideport Syringe To maintain the sideport syringe you can Inspect the syringe plunger seal Replace the syringe plunger Replace the removeable syringe needle Replace the syringe The sideport syringe plunger requires periodic replacement The frequency depends on the duty cycles the type of solvents being run through the syringe and the size of the syringe Replace the syringe plunger if it is leaking or damaged To either inspect or replace the sideport syringe plunger the syringe or the removable syringe needle complete the following steps Turn OFF the PAL power supply Move the PAL Injection unit to a clear position within the working space Loosen the plunger holder retaining screw 1 Unscrew the sideport syringe adapter screw 5 and remove the sideport syringe assembly from the Injection unit Loosen the two transfer tubing connection fittings 2 but do not remove them completely Loosen the plunger sealing screw 3 and lift it up 4 make sure the black Perfluor O ring remains in the plunger sealing screw Figure 50 Exchanging the Sideport Syringe Inspect the sideport syringe plunger and or the removeable needle and replace it if necessary To install the sideport syringe again repeat steps 1 7 81 Job Queue Job Cycle Method Method Parameters Object Trayholder Stack Tray
17. Manual 8 2 Svringe Priming 8 3 It is critical that syringes be primed before beginning sample preparation Prime the syringe by using the Utility function Clean Syr For fixed needle syringes priming may also be achieved by using an adequate number of filling strokes in a IFC PAL Method using the commands from the local terminal Gas tight syringes must be primed manually Remove the plunger and fill the syringe from the top of the barrel until solvent either overflows or forms a bead at the top of the syringe Then insert the plunger Installing a Syringe for the IFC PAL Injector Side Select Menu and press F1 Chang Syr The Injection Unit will move to a location that will facilitate installation of the syringe Place the syringe in the appropriate syringe adapter Pull the plunger out to approximately 20 of it s length Plunger Holder Syringe Adapter Figure 31 Syringe and Syringe adapter for IFC PAL Injector Side 55 IFC PAL User Manual 3 If necessary loosen the plunger retaining screw in the plunger holder see Figure 32 4 Move the syringe installed in the syringe adapter partially into the Injection Unit Guide the needle first into the upper needle guide and then into the lower needle guide 5 Place the plunger button into the plunger holder Allow the syringe adapter to dick into place by magnetic force against the syringe carrier 6 Tighten the plunger retaining screw against the plunger b
18. Support legs 45 IFC PAL User Manual 4 Screw the straining pieces together with the screws supplied Leave all screws a little loose try to lift the straining pieces into the final position and start tightening all screws over cross This procedure does ensure that the support legs are positioned parallel 5 Level out the IFC PAL frame by measuring the distance to the bench plate or by using a water level device If necessary make the required corrections with the adjustable legs from the supports note 78538378 ttis important that the frame is perfectly leveled out It will affect the gliding friction of the slider assembly 6 Mount the follower pin for the slider assembly at the left side of the slider device as shown in Figure 20 Figure 20 IFC PAL Assembling Tray Pan and X V Axis 7 Mount the X Y Axis on the support legs The same principle applies as described under point 6 1 2 Assembling the IFC PAL 8 Install the two Injection units as described under point 6 1 2 Assembling the IFC PAL 9 Install the two Keypad Terminals as described under point 6 1 2 Assembling the IFC PAL 46 IFC PAL User Manual 10 Install the Trav Pan starting from the left side where the holes are exactiv machined for the diameter of the of the pins The holes at the right side are wider to accept a certain dimension tolerance Move the slider assembly manually back and forth to ensure that the bearings are movin
19. follow the steps shown in Figure 48 Figure 48 Replacing the Injection Valve Valco Type W Remove the sample loop needle guide fitting and connection tubes from the valve body Unscrew to the hex screws which hold the valve to the valve drive Check that the valve guiding pin remains at it s position Install the replacement valve in the reverse order 78 OD IFC PAL User Manual Valve Rotor To replace and or clean the valve rotor follow the steps shown in Figure 49 Enlargement from the back Figure 49 Replacing Valve Rotor Valco Type W Do not remove the valve from the valve drive or any tubing or the loop Unscrew the knurled pre load assembly Do not tamper with the preset socket adjustment screw Engage the end of the rotor with a magnet or a pair of tweezers Locate the letter e g H stamped on the new or cleaned rotor and orient the letter to the lower half of the valve Insert the new rotor Make sure the rotor tab fits into the slot in the valve drive Replace the knurled pre load assembly Tighten the pre load assembly It must end up fully bottomed out 13 4 Injection Unit Follow the sequence of steps shown in chapter 6 2 Assembling the IFC PAL 13 5 Wash Station Follow the sequence of steps shown in chapter 6 2 Assembling the IFCPAL KO IFC PAL User Manual 14 Maintaining the IFC PAL System 14 1 General Maintance Regularly performing maintenance helps ensure accuracy and precisio
20. lithium batteries shall be disposed off locally according to national waste disposal regulations for batteries There are no operator serviceable parts on the electronic boards If an electronic board fails contact a CTC Analytics representative IFC PAL User Manual Commonly Used Symbols Electrical Power ON Used with Main PAL Power Supply Electrical Power OFF Used with Main PAL Power Supply Electrical Power ON for Only Part of the System Used with Optional Device s Electrical Power OFF for Only Part of the System Used with Optional Device s Caution Risk of Electrical shock high voltage HTS PAL Operating Manual General Information Printing Historv Safety Information Tables of Content A IFC PAL Operating Instructions Using the Control Terminal 1 Menu Screens 2 Function Keys 3 ESCape and STOP Keys 4 Scroll Knob and ENTER Button 2 Methods 2 1 Creating Methods 2 2 Edit View Methods 2 3 Delete Methods 3 Job and Job Queue 3 1 Building and Starting a Job Queue 3 2 Aborting a Job Queue 3 5 Restarting an Aborted Job Queue 4 Utility Functions 4 1 Syringe 42 Tray 4 3 Injector 4 4 Wash Station 4 5 Dilutor Side port Syringe for Collector Side B IFC PAL Description and Installation 5 General System Overview 5 1 IFC Pal used for Analytical Flow Rate Range 5 1 1 Specifications 5 2 IFC Pal used for Preparative Flow Rate Range 5 2 1 Specifications 5 3 Electrical Specifi
21. micro vials 1 0ml opposite side of 98 positions Tray Vial Tray 54 positions 6 X 9 for 12mm vials 2 0 ml 6 Trays may be used in Deep well Stack PAL Stack6DW Fraction Collector Vial Tray 21 positions 3 x 7 for 25 mm OD reagent tubes 150 mm height 55 ml Fraction Collector Vial Tray 39 positions 3 x 13 for 20 mm OD reagent tubes 150 mm height 35 ml Fraction Collector Vial Tray 50 positions 5 x 10 for 18 mm OD reagent tubes 150 mm height 27 ml Fraction Collector Vial Tray 50 positions 5 x 10 for 16 mm OD reagent tubes 150 mm height 16 ml Fraction Collector Vial Tray 78 positions 6 x 13 for 13 mm OD reagent tubes 150 mm height 9 ml 85 IFC PAL User Manual C Injection Cvcles HTS PAL LC Inj Cycle No Processing Step Method Parameter Object Class Used Object Value 1 Reference X Y Z axis and syringe System Start Ref ON plunger 2 Wait for Start signal Start Sync Signals 3 Read Barcode if enabled TRAY Tray Type Barcode None 4 Syringe wash strokes with solvent Pre Cln Slv1 SYRINGE Syringes Fill Speed from Wash1 Eject Speed Wash Wash Stations Needle Penetr Clean Volume Max Fill Speed Max Eject Speed 5 Syringe wash strokes with solvent Pre Cln Slv2 SYRINGE Syringes Fill Speed from Wash2 Eject Speed Wash2 Wash Stations Needle Penetr Clean Volume Max Fill Speed Max Eject Speed 6 Rinse syringe with sample select
22. pressure in inlet Poor reproducibility Syringe pressure differences when filling the syringe Reduce Inject Speed in method Increase Pullup Delay value Vacuum created in sample vial Reduce sample volume in sample vial High volatile solvent Use gastight syringe and sample tray cooling Increase Pullup Delay value Reduce Filling Speed in method Not properly crimped vials Excessive carryover between Dirty syringe and or valve injection port samples Check vial cap by attempting to rotate by hand Loose caps may cause selective loss of lighter components from sample Adjust crimping tool correctly Increase Pst Inj Slv1 and or Viv Cln Slv1 values in method Use PreClnSlv1 and PreClnSpl Waste tubing I D at Injection valve is too small causing waste liquid to be pulled back by capillary action into the rotor groove Replace the waste tubing with larger I D tubing Damaged or grooved valve rotor Replace valve rotor see chapter 13 3 Valve Rotor Valve needle seal leaks Inappropriate wash solvent Unexplained chromatographic Air is being introduced into the injection loop Needle peaks penetration depths may be inadequate causing air to be pulled into syringe Change Valve needle seal see chapter 9 2 Valve needle Guide Use appropriate wash solvent Check and or adjust Needle Penetration into sample vial see chapter 4 2 Make sure the Air Volume Method par
23. After pressing F1 either Wash1 or Wash2 may be used to clean the LC injection valve port without running a Job F2 Act Valve F2 switches the LC injection valve between the Load and Inject position It may be used to test the valve drive function or to perform manual injections F3 Movto In The Injection Unit moves to the injection valve position Bv selecting the Parameter Needle Penetr on the same screen the Injection Valve Needle Penetration value mav be checked or changed see chapter 9 3 F4 HOME The Injection Unit moves to its HOME position and the Job Queue Menu is displaved The following Injector Parameter may be changed by selecting the particular item Item Description Needle Penetr By selecting the Parameter Needle Penetr the Injection Valve Needle Penetration value may be checked and or changed To ensure reproducible sample injection and minimize carryover it is critical that the needle penetration depth is set accurately see chapter 9 3 Injection Valve Needle Penetration 25 IFC PAL User Manual 4 4 Wash Station After selecting the specific Wash Station the following Functions are available Function Key Description F2 Act Valve F2 switches the selected Wash Station valve between the Open and Close position It may be used to check the valve function or to prime the wash solvent lines F4 HOME The Injection Unit moves to its HOME position and the Job Queue Menu is displayed The following Wash Sta
24. Collector Side 1 Insert the sideport syringe without plunger into the syringe adapter Make sure the syringe side holes are adjusted to the left side 2 Locate the black connection fitting and screw it into the upper connection thread 3 Locate the white connection fitting and screw it into the lower connection thread 4 Put the plunger sealing screw over the syringe plunger 5 Put the black Perfluor O ring over the syringe plunger 6 Insert the plunger into the sideport syringe and carefully screw the plunger sealing screw into the syringe adapter bracket note _ t is important to follow the instructions step by step The sideport connections have to be tightened first to allow the syringe glass barrel to fell into the correct sealing position After this step one can continue with the step 4 as described above Do not over tighten the plunger sealing screw Check the plunger friction by manually moving the plunger up and down Loosen the plunger sealing screw if too much friction is applied Tr i L o Figure 34 Installing the Sideport Syringe for IFC PAL Collector Side 59 IFC PAL User Manual Ensure that the tubing kit connection fittings and it s guiding wire are attached properly to the sideport syringe adapter Also the syringe plunger must be inserted in the sideport syringe Turn OFF the PAL power supply Screw on the sideport syringe plunger
25. IFC PAL system to inject an analytical samples than all functions like the Method Job or Job Queue are relevant Job IFC PAL User Manual Using the Control Terminal The following procedures present the kev steps required to set up and process multiple groups of samples with the IFC PAL It is intended to provide an overview for new users and a reminder for infrequent users The IFC PAL and all accessories should be installed and Objects defined correctly A Syringe of the type called for in any Method to be used should also be installed Figure 1 illustrates the PAL Control Terminal and the conventions used to enter edit and view information JOB QUEUE ACTIVE 03 Stk1 01 001 amil 1 001 Figure 1 PAL Control Terminal and Conventions Menu Title Cursor bars highlight an item in a list Function Key Definitions Function Keys Press STOP to abort operation Press the inner knob to select an item highlighted by the cursor bars Press again to ENTER the selection Rotate the outer knob to move the cursor bars Press ESCape to return to the previous menu 1 1 IFC PAL User Manual Menu Screens Different menu screens are displayed depending on the HTS PAL operating state and the particular function being accessed by the operator All menu screens have the same basic format The menu title Is displayed at the top of the screen A list of items Is displayed below the title The date and time or a st
26. Manual Injection valve The IFC PAL can be equipped with different LC Injection valve types The recommended valve type for the IFC Pal is the Valco Vici Cheminert Type Valve In the Cheminert product range are valve types for specific applications available The Cheminert valve body is available made out of stainless steel or PEAK material PEEK related polymer For the various ranges of the flow rate are following bore sizes recommended Flow rate range 100 to 500 ul min Bore 0 25 mm Flow rate range 500 to 20 ml min Bore 0 40 mm standard Flow rate range 20 ml min Bore 0 75 mm These numbers shall be used as an orientation The valve selection depends also on the expected back pressure from the complete HPLC system All 3 valve types are delivers with standard Valco 1 16 inch connections lt is important to use original Valco Ferrules and Nuts to maintain a leak tight connection For the PEAK Valve only PEEK Ferrules can be used Stainless Steel Ferrules are too hard one can crack the PEAK Valve Stator by using the wrong ferule material The standard rotor material shipped is Valcon H with all valves made out of Stainless steel The PEAK Valve is equipped with a rotor made out of PEEK Teflon For special applications Is also a Vespel Polyimide rotor available This material is harder and the expected life time Is therefore shorter The selection of the rotor material depends directly from the application On custom
27. Tray Type IFC PAL User Manual Appendices Definition of Terms A Job Queue is a list of sample processing Jobs Jobs are executed in the order displayed on the JOB QUEUE menu screens New Jobs may be added to the queue while samples are being processed A Job contains the information needed by the PAL to process multiple samples by the same processing steps The elements of a Job are a Method and a Tray that defines the location of the samples to be processed For identification Jobs are automatically numbered from 01 to 99 and then restarting with 01 when they are added to the Job Queue A Cycle consist of the specific operations necessary to process one sample The Cycle operations are repeated for each sample within a Job Cycles are designed for specific applications The Standard HTS PAL Cycle is named LC In A Method defines how the samples are processed The elements of a Method are a Cycle a Syringe and a Parameter List Methods have names with up to 8 characters and can be edited copied and deleted Method Parameters are associated with the Cycle operations User assigned Parameter values define how a processing operation is performed A zero Parameter value will disable a Cycle operation Cycle parameters are application specific Objects are data structures describing the properties of physical modules Certain modules e g a Stack require several objects A Trayholder can hold one or more trays Each Trayholder ha
28. ack or Tray Cooler Peltier Version is described in the Addendum supplied with every unit If a Stack a Trayholder with multiple drawers was shipped with the IFC PAL loosen the two Torx screws on the two mounting clamps located on top of the Stack _ _ n 4 KAU Figure 16 Installing a Microplate Stack Carefully lift the X Crossrail assembly on top of the stack with the mounting clamp teeth fitting into the grooves on the bottom of the X Crossrail Be sure that the clamps fit completely into the grooves Alternately tighten the two Torx screws until the two mounting clamps are firmly in place Double check if the Stack clamps are correctly attached to the X Crossrail see Figure 6 Installing a Trayholder If a Trayholder was shipped with the IFC PAL loosen the two Torx screws on the two mounting clamps located on top of the Trayholder legs Figure 17 Installing a Trayholder 42 note l note l IFC PAL User Manual Install the Trayholder with the mounting clamp teeth fitting into the grooves on the bottom of the X Crossrail The Trayholder should be near the center of the X Crossrail Be sure that the clamps fit completely into the grooves Alternately tighten the two Torx screws until the two mounting clamps are firmly in place Double check if the two Trayholder clamps are correctly attached to the X Crossrail see Figure 5 page 19 6 1 3 Electrical connections Before defining the IFC PAL o
29. ameter is set to zero 1 Unexplained collisions of the Injection Unit Error Message Object Not Detected Object e g Travi LCVIvI Stk1 01 Error Message Object Collision before Z Tolerance Object e g Travi LCVIv1 Stk1 01 Error Message Motor AUX1 AUX2 failed IFC PAL User Manual Object s not defined correctly Incorrect Z value for the affected Object e g LC VIv1 Travi or Stack1 01 Define Object s correctiv see chapter 7 1 Defining Object Positions Redefine Z value for the affected Object see chapter 7 1 Defining Object positions Missing sample vial Deepwell or Microplate Incorrect Z value for the affected Object e g LC VIV1 Travi or Stack1 01 Injection valve drive not connected Insert sample vial Deepwell or Microplate Redefine Z value for the affected Object see chapter 7 1 Defining Object positions Switch OFF PAL and check connection between PAL and LC Viv see chapter 6 3 Defective LC Viv1 Connection cable Change connection cable MOTIO Board defective Replace MOTIO Board see chapter 13 1 MOTIO Board 72 note IFC PAL User Manual 13 Replacing Parts 13 1 MOTIO Board 1 Follow the sequence shown in Figure 43 to detach and release the MOTIO board from its position inside the X Crossrail 2 Carefully pull the two flat cable connectors upwards to free from the board 3 Install the replacement bo
30. ampering with or disconnecting these connections could endanger you and or damage the PAL System The instrument is properly grounded in accordance with these regulations when shipped You do not need to make any changes to the electrical connections or the instrument s chassis to ensure safe operation The combination of a PAL System with a LC MS System does require the safety measure as described by the LC MS System manufacturer Detailed instructions for the safety grounding on the LC MS system are outlined in the corresponding operating installation manual CTC Analytics recommends to use a grounding cable connected on one side at the Injection Valve Loop or any other suitable direct metallic contact and the other side at an appropriate grounding point at the LC MS System This supplementary grounding measure will support the safety strategy of the LC MS System manufacturer IFC PAL User Manual A Do not turn the instrument on if you suspect that it has incurred any kind of electrical damage Instead disconnect the power cord and contact a CTC Analytics representative for a product evaluation Do not attempt to use the instrument until it has been evaluated Electrical damage may have occurred if the PAL System shows visible signs of damage exposure to any liquids or has been transported under severe stress Damage can also result if the instrument is stored for prolonged periods under unfavorable conditions e g subjected to heat w
31. and OFF switch is accessible and easy to operate and where it is possible to unplug the AC power cord from the power supply wall outlet in case of emergency Other Hazards IFC PAL User Manual A To avoid injury during PAL System operation keep your hands away from the syringe A Do not operate the PAL System without the safety shield The safety shield must be installed for safe operation To avoid injury observe safe laboratory practice when you handle solvents change tubing or operate the PAL System Know the physical and chemical properties of the solvents you use See the Material Safety Sheets from the manufacturer for the solvents in use A Use caution when working with any polymer tubing under pressure e Always wear eye protection when near pressurized polymer tubing e Do not use polymer tubing that has been severely stressed or kinked e Do not use polymer tubing in particular not PEEK or Tefzel tubing with Tetrahydrofuran THF Dimethylsulfoxid DMSO chlorinated organic solvents concentrated mineral acids such as Nitric Phosphoric or Sulfuric acids or any related compounds to above listings Lithium batterv IFC PAL User Manual An onboard lithium battery buffers the electronic memories when the instrument Is turned off Replace it only with the same or equivalent type recommended by the equipment manufacturer Battery Panasonic VL 2330 soldered directly on the electronic board Discharged
32. ard in the reverse order After reconnecting the two flat cables to the board ensure that the cables are folded flat and can be slid inside the cross rail without damage Figure 43 Replacing MOTIO Board 153 IFC PAL User Manual 13 2 Control Board 1 Follow the sequence shown in Figure 44 to detach and release the Control board from its position inside the X Crossrail 2 Carefully pull the two flat cable connectors upwards to free from the board 3 Install the replacement board in the reverse order note l After reconnecting the two flat cables to the board ensure that the cables are folded flat and can be slid inside the cross rail without damage kul o o o 0 ME ma CUA KOM Figure 44 Replacing Control Board 74 IFC PAL User Manual 13 3 CPU Board 1 Remove the right end cover of the Crossrail facing the rear of the chassis 2 Slide the CPU board out and towards the right end of the Crossrail This Is necessary because the CPU board mates on its left side with a connector on the MOTIO board Eg 3 Install the replacement board in the reverse order INTERFACE INTERFACE 2 a INTERFACE INTERFACE 2 POWER uo gan BUS SEAS SERZ SERI Ka L me Figure 45 Replacing CPU Board 75 IFC PAL User Manual 13 4 Injection Valve and Valve Rotor 13 4 1 Standard LC Injection valve Valco VICI Cheminert Flat Plate Rotary Valve To replace and or clean the Ch
33. ater etc In any case disconnect the power cord s from the power supply or from the different power supplies if optional devices are installed before attempting any type of maintenance Capacitors inside the instrument may still be charged even if the instrument is turned off A To avoid damaging electrical parts do not disconnect an electrical assembly while power Is applied to the PAL system Once the power Is turned off wait approximately 30 seconds before you disconnect an assembly The instrument includes a number of integrated circuits These circuits may be damaged if exposed to excessive line voltage fluctuations and or power surges IFC PAL User Manual A Never try to repair or replace any components of the instrument that is not described in this manual without the assistance of a CTC Analytics representative There are no operator serviceable or replaceable parts inside the power supply ies or in the PAL System If a power supply Is not functioning contact a CTC Analytics representative A The power supply for the PAL Instrument has the symbols 1 0 on the label for the power switch to switch ON OFF Power ON 0 Power OFF If the basic PAL System is installed than a single power supply is installed only Turning OFF the power supply or pulling this single power cord in an emergency case will stop the complete PAL System lt is important that the power supply ies are in a location where the power ON
34. atus is shown in the highlighted area above the Function key labels on the bottom of the screen Menu Methods Method A SYRINGE 100u Air Volume Pre Cln 8lv1 Pre Cln Slv2 10 0 ul 100 pal 7 Deflt Figure 2 Accessing a Method Screen Function Keys Options for a particular menu are assigned to the corresponding function keys F1 F2 F3 and F4 directly below each function key label Pressing the function key defined as Home will always return to the Job Queue menu ESCape and STOP Keys Press the ESCape key to return to the previous menu Press the STOP key to abort the current Cycle Job or Job Queue Scroll Knob and ENTER Button Rotate the outer knob to scroll through items in a menu list To select a highlighted item press the central knob ENTER button Then use the outer knob to scroll through available options for that item or to change a numeric value Then press the inner knob again to ENTER the displayed option The inner knob is also used for other operations that require an ENTER operation to continue or complete an operation note l note l IFC PAL User Manual 2 Methods 2 1 Creating Methods Methods can be defined by the user and assigned names up to eight characters in length Methods can be created copied edited and viewed from the Method menu Methods can be viewed but not edited from the Job menu Methods are created by either copying an existing Method or creating a new Method
35. bject positions make sure the LC Injection Valve Fast Wash Station and the two Control Terminals are correctly connected to the IFC PAL X axis rear side The most common Objects for the IFC PAL Svstem like Injection valve Fast Wash Station and one Control Terminal are connected to the IFC Injector side Control Board To the IFC Collector side is typically only the second Control Terminal connected CPU and MOTIO Board Always switch OFF the PAL power supply before connecting or disconnecting any IFC PAL accessories cable 43 note l note l IFC PAL User Manual 6 2 IFC PAL Svstem Preparative Version 6 2 1 Unpacking the Components A ITS PAL System is shipped at least in two boxes One box contains the X Y Crossrail assembly the injection unit the keypad terminal standalone supports connecting cables power supply syringe kit the injection valve fast wash station assembly safety guard and miscellaneous parts The other box will typically contain Microplate Stacks and or Trayholders and Trays to hold reagent tubes for collection 1 Open the large box containing the X Y Crossrail First remove the Injection Units and the accessory boxes before attempting to remove the X Y Crossrail assembly 2 Remove any loose foam packing around the X Y Crossrail Carefully lift the X Y Crossrail and remove it from the box Hold the Y Crossrail in place as the assembly is removed from the box Set the X Y Crossrail assembly on a benc
36. cations 5 4 Physical Specifications 55 Operating and Environmental Requirements 6 Installation 6 1 IFC PAL Analytical Version 6 1 1 Unpacking the Components 6 1 2 Assembling 6 1 3 Electrical Connections IFC PAL User Manual GWO N 16 17 17 17 17 18 19 19 20 21 21 22 25 25 24 24 26 26 26 27 28 27 50 55 55 54 54 54 54 45 6 2 IFC PAL Preparative Version 6 2 1 Unpacking the Components 6 2 2 Assembling 7 IFC PAL Object Positions l 71 Defining Object Reference Positions _ 7 2 Description of Object Reference Positions 8 Syringes 8 1 Selecting Syringes 8 2 Syringe Priming 8 3 Installing a Syringe for the IFC PAL Injector Side 8 4 Removing a Syringe 8 5 Installing a Syringe for the IFC PAL Collector Side 8 6 Removing a Syringe 9 Injection Valve 9 1 Injection Valve Flow Path 9 2 Valve Needle Guide and Needle Seal 9 3 Injection Valve Needle Penetration 10 Interfacing the IFC PAL to other Devices 10 1 Synchronization and Output Signals 11 PAL Loader Program 11 1 Backing up the PAL Control Program 11 2 Reloading a Backup 12 Troubleshooting 13 Replacing Parts 13 1 MOTIO Board 13 2 Control Board 13 3 CPU Board 13 4 Injection Valve Valve Rotor 14 Maintaining the PAL System 14 1 General Maintenace 14 2 Maintaining Sideport Syringe IFC PAL User Manual 44 44 44 48 48 50 55 29 55 55 5 6 62 65 65 67 68 68 69 69
37. d 24 IFC PAL User Manual The following svringe parameters mav be changed bv selecting the particular item Item Syringe Syr Dilut Pos Dilutor Syr Prime Volume Pullup Del Fill Speed Eject Speed Eject Delay Description Indicates the type of sideport syringe currently used together with the dilutor module This parameter serves to define the dilute position of the sideport syringe plunger The position should be adjusted exactly above the lower hole of the sideport syringe It must be verified after every sideport syringe change Indicates the type size of dilutor syringe currently used The volume used to prime the solvent lines between the solvent bottle and the dilutor syringe and the transfer line between the dilutor syringe and the sideport syringe see page 18 FIPrime Using this item a delay time between solvent pullup and ejection while filling the dilutor syringe can be selected This feature is especially useful for handling viscous solvents Speed of dilutor syringe plunger movement used in all syringe filling operations Speed of dilutor syringe plunger movement used in all syringe eject operations Using this item a delay time between solvent eject and next solvent pullup of the dilutor syringe can be selected This feature is especially useful for handling viscous solvents 25 IFC PAL User Manual IFC PAL Description and Installation 5 General Svstem Overview 5 1
38. d Tray Holder e g THldr1 or Stack1 the X Y Z positions for the selected object will be displayed see Figure 24 Highlight the item Position X with the cursor bars and press ENTER The Injection Unit will move to the previous defined X axis position Rotate the outer knob to adjust the X axis position to the Trayholder Reference Position see Figure 23 Press the inner knob to ENTER the Position X value Repeat steps 3 5 for Position Y and Position Z Press the F3 button Moveto Zero The Injection Unit will move to the HOME position Verity the defined X Y Z Positions by pressing FI Check Pos 49 IFC PAL User Manual 7 2 Description of Object Reference Positions Trayholder e g THIdr1 Figure 25 Trayholder Reference Position For Trayholder the Reference Position is a hole in the base plate of the Holder The lower needle guide should be centered in the hole with the bottom of the needle guide flush with the bottom of the base plate Trayholder with six or three drawers e g Stack1 Figure 26 Stack Reference Position For a six drawer Stack the reference position is a hole located in the second drawer see Figure 26 For a three drawer Stack the reference position Is in the first top drawer see Figure 26 The lower needle guide must be centered in the hole with the bottom of the needle guide flush with the bottom of the drawer The same logic applies as well to Stack or Tray Coolers For details se
39. d Volume for changes Collect Waste in ul range Injection cycle time Typically 20 60 sec depending on plunger speeds injection volume and wash cycles 2 IFC PAL User Manual 5 2 IFC PAL Used for Preparative Flow Rate Range Typically 1 to 100ml min Figure 5 IFC PAL Major System Components for Preparative Version The IFC PAL configuration can include at the Injector side a Trayholder Microplate Stack Peltier cooled or not cooled a 6 port LC Injection Valve prep range and a Fast Wash Station At the Collector side can various types of Trayholders be installed to keep reagent tubes from 13 to 25 mm OD In addition a second valve drive analytical range can be added An optional slider is available to hold standard racks designed for a Gilson System 28 IFC PAL User Manual 5 2 1 Specifications for IFC PAL Preparative Version General Specifications Sample Capacitv Injector Side 98 x 2ml vials per Tray 200 x Iml vials per Tray 32 x 10ml 20ml vials per Tray Thermostatted Sample Tray Optional 4 C 70 C 6 Deepwell or Standard Microtiterplates in a 3 drawer Stack 12 Standard Microtiterplates in a 6 drawer Stack Injection volume range 100 250 500 1000 2500 and 5000 ul syringes are available Maximum injection volume 20 ml 4 x 5ml Loop Volume Range Loops up to 20 ml are available Replicate injections 1 99 from one vial Wash Station 2 different wash solvents Precision Typically lt
40. e manner a sturdy cardboard box can be used before attempting to install the legs 3 Install the legs near the ends of the X Crossrail Loosen the Torx screws on the mounting clamps and then fit one leg into the grooves in the X Crossrail Be sure that the clamps fit completely into the grooves Tighten the Torx screws until the legs are firmly in place 4 Double check if the legs and stack claws are correctly attached to the X Crossrail see Figure 6 following page 54 IFC PAL User Manual Figure 6 Attachment of Mounting Claws Installing the Injection Unit note __ nstallation of the Injection Unit should be done carefully When installing it for the first time have someone hold it in place while the mounting screws are inserted see Figure 8 4 D Guiding Pins Figure 7 Attaching the PAL Injection Unit 1 Remove the 3 Torx mounting screws A B and C that will be used to fix the Injection Unit to the Y Crossrail Place one of the screws onto the end of the supplied Torx driver Slide the clear plastic cover on the Injection Unit all the way to the top 55 IFC PAL User Manual 2 Connect the flat ribbon cable A protruding from the front end of the Y Crossrail to the corresponding connector on the Injection Unit see Figure 8 A Guide plug into socket B Guiding pins into guiding holes Figure 8 Connecting the Injection Unit Flat Cable 3 Hold the Injection Unit in place against the Y C
41. e syringe detection system is set to manual the extension man is displayed This value can not be changed This parameter serves to control the filling of the syringe It may happen that air bubbles remain below the plunger after the first pull up If the plunger is moved up and down several times see Fill Strokes these air bubbles are worked out With this operation the syringe may be completely filled even when using very small sample volumes Number of Fill Strokes All Fill Strokes except the last one use the selected Fill Volume If the selected Sample volume is higher than the Fill Volume the Sample Volume Is used for all Fill Strokes If zero is selected the plunger is pulled up only once using the Sample volume value Using this item a delay time between sample pullup and ejection while filling the syringe can be selected The same delay time is used after the last plunger pullup until the syringe needle is moved out of the sample vial well It is only used if more than one Fill Stroke is selected This feature is especially useful for handling viscous fluids or syringe sizes P100ul Speed of plunger movement used in all syringe filling operations Speed of plunger movement used in all syringe eject operations except sample injection Speed of plunger movement for sample injection Plunger position during Chang Syringe operation The syringe plunger is moved to a position where the syringe can be removed and replaced
42. e the specific manual Addendum supplied with every unit 50 note l note l IFC PAL User Manual Figure 27 Fast Wash Station Reference Positions For a Fast Wash Station the reference positions are two holes above the Wash Station glass liners see Figure 27 Wash and Wash2 The lower needle guide should be centered in these holes with the bottom of the lower needle guide lightly touching the surface of the Wash Station assembly The Waste position represents an Injector within the PAL software It is defined in the Object class Injectors see Fig 28 Injectors e g LC Vivi or Waste Figure 28 LC Valve and Waste Reference Position For an LC Valve the reference position is the valve needle guide fitting mounted on the top valve port see Figure 28 The lower needle guide of the Injection Unit should be centered In the valve needle guide fitting Adjust the Z Position that the bottom of the lower needle guide Is just touching the surface of the valve needle guide fitting Then reduce the value by 2 0 mm For the Waste Port the reference position Is a hole slightly larger than the needle guide in front of Wash2 see Figure 27 The lower needle guide should be centered in this hole with the bottom of the lower needle guide lightly touching the surface of the Wash Station assembly To adjust the Valve Needle Penetration value see chapter 9 3 5 Safetv Warning l IFC PAL User Manual Follower Pin for Sl
43. ected to this point 52 Note l 8 1 IFC PAL User Manual Svringes Selecting Svringes Recommended Syringe for the IFC PAL for analytical application Injection Side 1 PAL SyrLC100ul Kit LC Syringe 100ul for HTS PAL consisting of 1 pc syringe adapter 1 pc plunger holder 2 pc syringe SYRC G100 22S 3 The SYRC G100 225 3 gastight Syringe for IFC PAL equipped with 22S gauge needle Is appropriate for injection into the standard CTC injection valve However certain applications may require different syringe sizes or needle ID Consult the PAL Accessories Catalog Recommended Syringe for the IFC PAL for preparative application Injection Side 1 PAL SvrPrep5000ul Kit LC Syringe 5 0 ml for IFC PAL consisting of 1 pc syringe adapter 1 pc plunger holder 2 pc syringe SYRC G5000 19 3 The SYRC G5000 19 3 gastight Syringe for IFC PAL equipped with 19 gauge needle is appropriate for injection into the CTC prep injection valve However certain applications may require different syringe sizes or needle ID Consult the PAL Accessories Catalog The Needle Dimension for Gauge 19 is OD 1 07 ID 0 69 mm The needle guides hole for needle from the injection are adjusted with new delivered units Existing units in the field may have to be upgraded The Fast Wash Station P N MM 01 04F has to have glass liners with an internal diameter of 1 50 mm Needle Guide and Needle Seal from the injection valve have to be adapted to Gau
44. ed zIp format and extracted into the sss file which is the PAL Loader format Complete the following steps to reload a PAL backup Shut off power to the PAL and the computer Connect the grey null modem cable between the PAL SER1 and a PC serial port Switch on power to the PAL When the PAL Job Menu is displayed start up the computer Double click the PAL Loader icon the PAL Loader screen appears Click the Update button Click the Browse button and select the appropriate sss backup file Click the Open button The Update Flash Memory window will be displayed The path and filename for the update file will be shown in the Filename entry box Click the Update button to load the new firmware The process will take several minutes If the update Is successfully completed the message Update of target memory succeeded will be displayed Click the Close button to exit the Backup dialog box Click the Start PAL button to terminate control by the Loader program On the Keypad terminal the Job Queue screen IS displayed Disconnect the RS 232 cable from the PAL 70 IFC PAL User Manual 12 Troubleshooting note l The HTS PAL represents always one of several components in a chromatography system The following Troubleshooting Guide is limited to the HTS PAL only Symptom or Error Message Possible Cause No or very low detector signal The valve needle guide and or needle seal are not is ob
45. ed Pre Cln Spl SYRINGE Syringes Eject Speed number of times Sample Volume Fill Volume Fill Speed TRAY Tray Type Needle Penetr Pullup Delay Waste Injectors Needle Penetr 7 Fill syringe with sample using Sample Volume SYRINGE Syringes Eject Speed several filling strokes aspirate air Air Volume Overfill outside of vial if Air Volume 7 0 Fill Speed Fill Volume Fill Strokes TRAY Tray Type Needle Penetr Pullup Del 8 Move to injection valve Inject to 9 Wait for Inject signal Inject Sync Signals 10 Drive needle to penetration depth Inject to Injectors Needle Penetr 11 Delay Pre Inj Del 12 Switch valve to Active position 15 Activate Injected signal Injected Out Signals Pulse Time 14 Activate Injectd Signal 15 Dispense syringe contents into Inject Speed sample loop 16 Delay Pst Inj Del 17 Switch valve to Standby position 18 Retract needle from injector 19 Clean syringe and needle with Pst Cln Slv1 SYRINGE Syringes Fill Speed solvent from Wash1 Eject Speed Wash Wash Stations Needle Penetr Clean Volume Max Fill Speed Max Eject Speed 84 IFC PAL User Manual 20 Clean svringe and needle with solvent from Wash2 SYRINGE Syringes Fill Speed Eject Speed Needle Penetr Clean Volume Max Fill Speed Max Eject Speed 21 Rinse valve inlet with solvent from Wash1 SYRINGE Syringes Fill Speed Inject Speed Needle Penetr Clean Volume Max Fill Speed Max Eject Speed 22 Rinse valve inlet wi
46. eminert injection valve follow the steps as shown in Figure 46 Figure 46 Replacing the Standard LC Injection Valve Valco VICI Cheminert 1 Remove the sample loop needle guide fitting and connection tubes from the valve body See Figure 35 left picture It is a good practice to label the connection tubes before removal 2 Unscrew to the hex screw which holds the valve to the valve drive 3 Check that the valve guiding pin remains at it s position 4 Install the replacement valve in the reverse order 76 note l IFC PAL User Manual Valve Rotor LC Standard Valve Valco VICI Cheminert Flat Plate Rotarv Valve To replace and or clean the Cheminert valve rotor follow the steps shown in Figure 47 Figure 47 Replacing Cheminert Valve Rotor Unscrew the two hex screws retaining the stator Remove the old rotor with an appropriate tool If necessary clean the surfaces without scratching the metal parts Insert the new rotor press the polymer disk carefully into position Put the stator back on tighten the two hex screws The valve is ready for use at the factory set pressure In the event of damage of the stator replacements or factory refinishing are available The rotor material is Valcon H for HPLC use The type of material is not marked on the valve 7 B UNN IFC PAL User Manual 13 4 20ptional Injection Valve Type W and Valve Rotor Injection valve Type W To replace and or clean the injection valve
47. ers demand CTC Analytics can also supply the Valco W Type valve This type is only available in stainless steel with a standard bore of 0 40 mm The injection loops are available in a wide range from 10 to 5000 ul All loops have a 1 16 inch tubing at the connection point The 2 loops for 2 5 and 5 ml have 1 16 inch connections but the tubing Is widened up to 1 8 inch to eliminate a too high back pressure 62 IFC PAL User Manual 9 1 Iniection Valve Flow Path 9 1 1 Injection Valve Flow Path for Valco VICI Cheminert Valve Type p Sample Loop M Carrier mobile phase Figure 37 Standard LC Injection Valve Flow Path Valco VICI Cheminert Valve The standard LC Injection Valve is a 6 port two way switching Valve with a special needle guide Valco VICI Cheminert Flat Plate Rotary Valve Stator Material Stainless steel 316 Rotor Material Valcon H inert mix polymer standard can be replaced by other material Port Size 1 16 inch Fittings Valco 1 16 inch Ferrules and Nuts Actuator Micro Electric Actuator 63 IFC PAL User Manual 9 1 2 Injection Valve Flow Path for Valco Valve Type W af d in II Sample Loop AEI vici Ge WA 7 we Vent waste 6 o Carrier mobile phase Figure 38 LC Injection Valve Flow Path for Valco Valve Type W The LC Injection valve Valco Type W Conical Rotary Valves 6 port two way switching valve with the special needle guide Stator Mate
48. es Part RS3M 2000 and the AC power cable 2 Set the power supply switch to the OFF position 3 Connect one end of the DC power cables to the power supply in the connector PAL and AUX and the other ends to the POWER connectors at the rear side of the X Crossrall 4 Connect the female end of the AC power cable to the power supply Then connect the male end to an AC power outlet 5 Set the switch on the power supply to the ON position 6 Observe the Keypads display The model name IFC PAL Injector and IFC PAL Collector will be displayed along with the software version number The Job Queue menu screen will then be displayed note Before proceeding with the remaining steps switch OFF power to the IFC PAL 38 IFC PAL User Manual Installing the LC Injection Valve 1 Locate the blue valve drive It will have one clamp that is identical to other object clamps Loosen the clamp as above see Figure 12 Figure 12 Installing the Injection Valve Drive 2 Attach the valve drive to the X Crossrail and tighten the mounting screw note To avoid unnecessary delay volume between sample injection point and detection the injection valve should be located near the detection device 3 Connect the control cable from the valve drive to AUXI at the rear of injector IFC PAL Side 4 The injection valve and rotor Is pre installed on the valve drive 39 IFC PAL User Ma
49. g without any friction 11 Install the safety shield in front of the slider assembly as shown in Figure 20 Figure 22 IFC PAL Assembly as an example configuration 4 note l 7 1 IFC PAL User Manual IFC PAL Object Positions Defining Object Reference Positions Remove the Svringe Adapter from the Injection Unit before performing the following steps The objective is to define the Reference Positions for standard IFC PAL Objects Make sure the Trayholder s Valve s and Fast Wash Station are properly mounted to the PAL X axis The following description is an example how to teach the Reference Position for a Trayholder The described procedure is common to all IFC PAL Objects Fig 23 Object Reference Position For Trayholder the Reference Position is a hole slightly larger than the lower needle guide in the base plate of the Holder The lower needle guide should be centered in the hole with the bottom of the needle guide flush with the bottom of the base plate Switch ON the IFC PAL power supply When the Job Queue menu Is displayed complete the following sequence common to all objects Menu Setup Objects Tray Holders Named Tray Holder where Named Tray Holder represents a predefined Trayholder e g THldr1 or Stack1 48 IFC PAL User Manual Tray Holder THldr1 1998 08 51 11 20 25 Check Clear Movto Fos Pos Pos Figure 24 Menu Screen Object Trayholder After selecting Name
50. g step Output Signals Out Signals are sent from the PAL to external devices to indicate status or completion of particular processing steps These signals are classified as Objects Physical Events e g TTL In1 are also Objects and may be assigned to named signals PAL Cycles require that certain signals such as Start Inject and Injected be defined See Table below for the PAL Events and signal assignments associated with the standard PAL LC Inj Cycle can be used for the IFC PAL System or for an isolated injection cycle The Synchronization Signal shall be set at the IFC PAL Injection Side only The dedicated IFC PAL Software will start the Collector side accordingly To assign a physical Event e g SW Out 1 to an existing signal Object Injected complete the following menu selections Out Signals Injected Destination SW Outi PAL s are shipped with all Cycle events pre defined as shown in the table below If a different physical signal needs to be used then it will be necessary to assign a new Event to the signal Object If a signal Is to be ignored then it s corresponding Event must be set to Immediat Standard Assignment for IFC PAL Description Default INTERFACE Injection Cycles Events Pin Start Sync Signal Start a cycle Input from LC or TIL InI ii data system 8 GND Inject Svnc Signal Inject Immediat READY to INJECT Ignore Injected Out Signal Is activated atthe moment when SW O
51. ge 19 See Chapter 9 55 IFC PAL User Manual Recommended Svringe for the IFC PAL for Collector Side Analvtical Version 1 PAL SyrLCSP20ul Kit Dilutor Syringe for IFC PAL consisting of 1 pc sideport syringe adapter 1 pc sideport plunger holder 1 pc sideport syringe plunger sealing Screw 1 pc sideport syringe 20ul SYRC Sp20 R 3 pc needles gauge 225 for sideport syringe Ndl S 22S 3 The sideport syringe is used to divert the effluent flow from the HPLC column detector to Collect or Waste The needles are replaceable The recommended needle is appropriate for injection into the CTC injection valve However certain applications may require different syringe sizes or needle ID Consult the PAL Accessories Catalog Recommended Syringe for the IFC PAL for Collector Side Preparative Version 1 PAL SyrLCSP80ul Kit Dilutor Syringe for IFC PAL consisting of 1 pc sideport syringe adapter 1 pc sideport plunger holder 1 pc sideport syringe plunger sealing Screw 1 pc sideport syringe 80 SYRC Sp80 R 3 pc needles gauge 19 for sideport syringe Ndl L 193 The sideport syringe is used to divert the effluent flow from the HPLC column detector to Collect or Waste The needles are replaceable The recommended needle is appropriate for injection into the CTC prep injection valve However certain applications may require different syringe sizes or needle ID Consult the PAL Accessories Catalog 54 IFC PAL User
52. h and remove the foam pieces from each end 3 Unpack the remaining small boxes and any other containers 4 Place the IFC PAL onto a stable surface Make sure that no objects will interfere with either the Y Crossrail or Injection Unit throughout the entire range of potential movements 6 2 2 Assembling The assembling steps described are for the specific preparative parts of the IFC PAL system Assembling of the support legs for the slider plate The assembling with standard objects like the Injection valve Fast Wash Station Trayholder Stacks etc is described above under point 6 1 in the section for the analytical version lt is important that the IFC PAL for the preparative application is mounted on a solid bench plate The bench has to be leveled and has to have a smooth surface 44 IFC PAL User Manual Installing the Support and Slider Assembly Open the transport locking screw using the supplied Allen Key See Figure 18 Figure 18 IFC PAL Support Leg Transport Lock Position the two support legs parallel to each other on the table with approximately 57 cm distance in between the two legs The support leg with the sensor cable installed at the back side has to be on the left side Position the two straining pieces in between the two support legs Adjust the distance in between as perfect as possible to ensure that the support legs are running parallel to each other Figure 19 IFC PAL Straining of
53. holder into the black Injection unit slider Figure 35 Installing the Sideport Syringe plunger holder for IFC PALCollector Side Pull out the plunger to approximately 20 of it s length If necessary loosen the plunger retaining screw in the plunger holder Move the syringe installed in the syringe adapter partially into the Injection Unit Guide the needle first into the upper needle guide and then into the lower needle guide Guide the syringe adapter side bracket through the left hand Injection unit slit 60 note l 14 15 16 IFC PAL User Manual Place the plunger button into the plunger holder Allow the syringe adapter to dick into place by magnetic force against the syringe carrier Tighten the plunger retaining screw against the plunger button Tighten the sideport syringe adapter screw against the black Injection unit slider Figure 36 Installing the Sideport Syringe Adapter for IFC PAL Collector Side Turn ON the PAL power supply During the syringe initialization process the plunger moves down until it hits the mechanical stop This position Is stored as the syringes zero volume position 8 6 After replacing a sideport syringe in a IFC PAL System always check the plunger position as described in Utilities Functions Syr Dilut Pos Removing the Sideport Syringe Adapter for IFC PAL Collector Side Repeat steps 1 17 in chapter 8 5 in reverse order 61 IFC PAL User
54. ical power plug b Over Voltage Category Il Over Voltage category II pertains to instruments that receive their electrical power from a local level such as an electrical wall outlet c Pollution Degree2 This Is a measure of pollution on electrical circuits that may produce a reduction of the dielectric strength or surface resistivity Degree 2 refers to normally only non conductive pollution Occasionally however a temporary conductivity caused by condensation must be expected d Moisture Protection Normal IPXO IPXO means that there is NO Ingress Protection against any type of dripping or sprayed water The X Is a place holder to identify protection against dust if applicable 50 IFC PAL User Manual Electrical Specifications Continued Parameter Requirements U W tbwcgCfl H PAL System AA E PAL System Power Supply SSS a PAL Single Valve Module Serial Control PAL Single 2 Valve 3 Valve Module Optional Devices PAL Valve Module Power Supply Serial control Single 2 Valve 3 Valve Module Optional Devices aa A A AA Stack Cooler DW MT or Trav Cooler Peltier Element Optional Devices Input Voltage 24 VDC Input Current DAG GG CF Power Supply for Stack Cooler DW MT or Tray Cooler Peltier Element Optional Devices 51 IFC PAL User Manual Electrical Specifications Continued PAL IFC Box Interface Box for Fraction Collector A D Converter Optional
55. ider Assembly Preparative Version Figure 29 Follower Pin for Slider Assembly Preparative Version The reference position for the Follower Pin of the Slider Assembly is the hole at the top of the tube See Figure 29 Adjust the Z Position of the lower needle guide such that it does enter into the hole The higher rim at the back side of the tube has to be in contact with the lower needle guide The cut out in the front of the Follower Pin is reserved for the needle If longer needles are used the cut out has to be mechanical changed Waste Position for Slider Assembly Preparative Version ot Figure 30 Waste Position for Slider Assembly Preparative Version For the Waste Port the reference position Is a hole slightly larger than the needle guide in front of Wash2 see Figure 30 The lower needle guide should be centered in this hole with the bottom of the lower needle guide lightly touching the surface of the Wash Station assembly This waste port Is used for clean up procedures at a stop or abort action The wire of the transfer tubing is connected to the screw at the front of the clam The IFC PAL System used for preparative application has to be grounded with special care Organic solvents can be electrostatic charged resulting sparks can start a fire hazard The screw connection mounted at the rear side of the clam is used for electrical grounding The grounding cable from laboratory has to be conn
56. jection Units and the accessory boxes before attempting to remove the X Y Crossrail assembly 2 Remove any loose foam packing around the X Y Crossrail Carefully lift the X Y Crossrail and remove it from the box Hold the Y Crossrail in place as the assembly is removed from the box Set the X Y Crossrail assembly on a bench and remove the foam pieces from each end 3 Unpack the remaining small boxes and any other containers 4 Place the IFC PAL onto a stable surface Make sure that no objects will interfere with either the Y Crossrail or Injection Unit throughout the entire range of potential movements 6 1 2 Assembling The assembling steps are described as an example for a single injection unit Apply the same steps If a second unit is required for the IFC PAL System as well Before beginning the assembly process determine approximately where the LC injection valve will be located The 2 control terminals will be mounted on either side of the X Crossrail 1 Ifa Stack a Trayholder with multiple drawers was shipped with the IFC PAL loosen the Torx screws on the two mounting clamps located on top of the stack 2 Move the Y Crossrail to the center of the X Crossrail and temporarily place the X Crossrail assembly on top of the stack with the mounting clamp teeth fitting into the grooves on the bottom of the X Crossrail The stack should be near the center of the Crossrail For IFC PAL s without a Stack support the Crossrail in a suitabl
57. n of the PAL System Suggested intervals for maintenance procedures to ensure uninterrupted operation are given below If you use the system heavily for example nights and weekends or if you use aggressive solvents you may need to perform the maintenance procedure more frequently Clean the outside of the instrument Use only a soft lint free paper or cloth dampened with mild soap and water Clean Instrument syringe and surfaces Weekly or as needed Every 1500 to 2000 penetrations RGD ace 71G ka Meade ea Check the tightness of the needle in the needle seal Replace the valve rotor Annually or more a year depending on the throughput and quality of the sample solution and Mobile Phase Syringe Plunger has to be replaced on a regular base The interval is highly dependent on the application throughput quality of sample solution particles etc washing solvent It is advisable to check the tightness of the plunger on a regular base to gain the experience with the own application Weekly or as needed Replace the valve rotor Replace the syringe plunger The other steps are described in the Preventative Maintenance Procedure Specific kits for the GC or the HPLC techniques are available The kits include the parts which shall be changed annually PM Kit1 for HPLC and PM Kit2 for GC technique note l There are no operator serviceable or replaceable parts inside the power supply ies or the PAL System
58. nual Installing the Fast Wash Station Attach the Wash Station assembly to the Solvent bottle holder Figure 13 Installing the Fast Wash Station Loosen the screw on the Fast Wash Station mounting clamp Attach the Fast Wash Station to the X Crossrail as close as possible to the Injection Valve This will minimize the time required to move between the two positions Tighten the mounting screw Figure 14 Fast Wash Station Assembly 40 note l IFC PAL User Manual Locate the white Teflon fittings and two lengths of Teflon tubing that connect the Wash Station valves to the wash solvent reservoirs Place the reservoirs onto their holders and attach the tubing and fittings Attach one end of the supplied transparent Polvethvlene tubing to the Wash station waste port Place the other end of tubing into a waste reservoir not supplied which is lower positioned than the Wash station assembly Stretch the Polyethylene tubing to make sure that no used wash solvent is trapped before the Waste Reservolr The waste reservoir MUST be placed in a lower position than the Wash Station assembly Connect the control cable to the connector Wash Station at the rear side Control Board and the four pronged connector located on the Fast Wash Station assembly Figure 15 Electrical Connection Fast Wash Station 4 note l IFC PAL User Manual Installing a Microplate Stack Installation and operation of a St
59. on Object Reference Position Menu Screen Object Trayholder Trayholder Reference Position Stack Reference Position Fast Wash Station Reference Positions LC Valve and Waste Reference Position Follower Pin for Slider Assembly Preparative Version Waste Position for Slider Assembly Preparative Version Syringe and Syringe Adapter Installing and Removing a Syringe from the IFC PAL Injector Side Attaching the Transfer Tubing Kit Installing the Sideport Syringe from the IFC PAL Collector Side Installing the Sideport Syringe Plunger Holder Installing the Sideport Syringe Adapter IFC PAL User Manual 16 20 26 28 55 55 56 57 57 58 39 40 40 4 42 42 45 45 46 4 4 48 49 50 50 51 51 52 52 55 58 59 60 61 Figure 37 Figure 38 Figure 39 Figure 40 Figure 41 Figure 42 Figure 43 Figure 44 Figure 45 Figure 46 Figure 47 Figure 48 Figure 49 Figure 50 LC Injection Valve Flow Path Cheminert Valve LC Injection Valve Flow Path Valve Type W Valve Needle Guide and Seal Menu Screen Valve Needle Penetration Depth PAL Loader Menu Screen PAL Loader Backup Target Memory Replacing MOTIO Board Replacing Control Board Replacing CPU Board Replacing Injection Valve Cheminert Type Replacing Valve Rotor Cheminert Type Replacing Injection Valve Type W Replacing Valve Rotor Type W Exchanging the Sideport Syringe IFC PAL User Manual 65 64 65 6 7 69 69 13 74 75 76 li 78 19 81 note l
60. ons selectable from the Menu screen provide quick access to checking operations and parameters that may need to be changed These functions are available for the actual Syringe Trays Injectors and Wash Stations They allow access to key functions without having to set up and execute a Method and Job If an item is used in the sample processing cycle the appropriate Utility value will be overwritten by the Method value Syringes By pressing a Function Key the following functions are available Function Key F1 Chang Syr F2 Clean Syr F3 Set Pos F4 HOME Description The syringe is moved to a position where the syringe assembly can be completely lowered to facilitate removal of the syringe adapter The syringe can then be removed and replaced A prompt will be displayed to specify the new syringe The syringe must be installed before pressing Enter see Chapter 8 Syringes This Function is used to clean or prime the syringe prior use After selecting F2 either Wash1 or Wash2 can be selected Set Pos is used to define the Chang Syringe position The Injection Unit moves to its HOME position and the Job Queue Menu is displayed The following Syringe Parameters may be changed by selecting the particular item Item Actual Id Fill Volume Fill Strokes Pullup Del Fill Speed Eject Speed Inject Speed Plunger Pos Description Indicates the Identification number ID of the currently inserted syringe If th
61. rial Stainless steel 316 Rotor Material Valcon H inert mix polymer standard can be replace by other material Port Size 1 16 inch Fittings Valco 1 16 inch Ferrules and Nuts Actuator Micro Electric Actuator note Sample loops of the two different valves are not interchangeable 64 IFC PAL User Manual 9 2 Valve Needle Guide and Needle Seal The two valves are equipped with a special valve needle guide fitting This fitting has a wide diameter to mate with the syringe needle guide on the injection unit The valve needle guide also has a countersunk hole to facilitate insertion of the syringe needle into the injection port Valve Needle Guide Valve Needle Seal _ Figure 39 Valve Needle Guide and Valve Needle Seal Example Valco VICI Cheminert Valve Needle Guide and seal for Valco Valve type W is identical Following Needle Guides are available P N MV 30 12 Needle Guide stainless steel for Gauge 22 needles P N MV 30 16 Needle Guide PEEK for Gauge 22 needles P N MV 30 52 Needle Guide stainless steel for Gauge 19 needles marked with a groove at outer rim 65 IFC PAL User Manual The valve needle guide holds the needle seal The needle seal which is a short length of Teflon tubing forms the seal around the syringe needle A stainless steel ferrule is tightened around the Teflon sleeve to ensure a leak proof fit Following Needle Seals are available package of 10 seals
62. rossrail Make sure the two locating pins on the Y Crossrail fit into the two guiding pin holes on the Injection Unit 56 IFC PAL User Manual Locate the three large holes in the black anodized frame attached to the Z Crossrail inside the Injection Unit Slide the frame upwards until the top hole is centered on the top threaded hole in the end of the Y Crossrail Insert and securely tighten the Torx screw A see Figure 9 Figure 9 Inserting the Injection Unit Mounting Torx Screws Install the two remaining Torx screws B C in the left and right mounting holes respectively It may be necessary to move the elastic cord slightly to the left to insert the Torx screw C into the right hand hole Figure 10 IFC PAL with Injection Unit and Standalone Supports only 1 injection unit shown 57 IFC PAL User Manual Installing the Kevpad Terminals and Safetv Shield Sa Figure 11 Installing Keypad Terminals 1 Install the Safety Shield on the left and right sides to the outside of the X Axis 2 Install the Keypad mounting brackets on the right and left side of the X Crossrail 3 Connect one end of the white coiled cables Part SS8J 700 to the Keypad and the other end to the two SER3 interfaces jack on the rear side of the X Crossrail 4 Place the Keypad terminals onto it s mounting brackets Installing the Power Supply 1 Locate the power supply the DC power cabl
63. s a reference position X Y Z co ordinates that defines it s location A Stack Is a particular type of Trayholder that is designed to hold micro plates A six drawer Stack holds 12 standard micro plates two in each drawer A three drawer Stack holds six deep well micro plates two in each drawer A Tray that holds multiple samples Trays are defined by designating the Tray Type see below and the Trayholder Tray names are used to identify the sample source within a PAL Job A Tray Type defines the pattern and sampling sequence of sample locations within a Tray Standard Tray Types include shallow and deep well 96 position Microplates and Trays that hold 1 2 10 and 20ml vials 82 IFC PAL User Manual Conventions of Naming This section recommends standard naming conventions for HTS PAL Travs Trav Tvpes and Trav holders Following these conventions will allow HTS PAL s to be pre configured for certain applications will simplify software backups and application development and will improve technical support and training Tray Type MT96 DW96 M1384 V1200 VT98 VT78 V154 FC21 55 BELLS FCS 27 FC50 16 FC 78 09 Tray Description Standard 96 position microplates Deep well 96 position microplates High density 384 position microplates Vial Tray 200 positions 10 X 20 for 7mm micro vials 1 0 ml Vial Tray 98 positions 7 X 14 for 12mm vials 2 0 ml Vial Tray 78 positions 6 X 13 for 7mm
64. ser s authority to operate the equipment The user shall be made aware that if the equipment is used in a manner not specified by the manufacturer the protection provided by the equipment my be impaired When you use the PAL System follow the generally accepted procedures for quality control and methods development When you use the PAL System in the field of chromatographic analysis and you observe a change in the retention of a particular compound in the resolution between two compounds or in peak shape immediately determine the reason for the changes Until you determine the cause of a change do not rely on the separation results Electrical Hazards IFC PAL User Manual Every analytical instrument has specific hazards so be sure to read and comply with the following precautions They will help ensure the safe long term use of your PAL System The Installation Category Over voltage Category for this instrument is Level Il The Level Il Category pertains to equipment that receives its electrical power from the local level such as an electrical wall outlet Only use fuses of the type and current rating specified Do not use repaired fuses and do not short circuit the fuse holder The supplied power cord must be inserted into a power outlet with a protective earth contact ground When using an extension cord make sure that the cord also has an earth contact Do not change the external or internal grounding connections T
65. served properly installed Recommended Action Check valve needle guide and seal see chapter 9 2 Valve Needle Guide The valve ports are not plumbed correctiv to the pump and or detection svstem Check plumbing connections see chapter 9 1 Injection valve flow path Wrong valve tvpe specified Check valve type by pressing Menu Setup Objects Injectors LC VIv1 Valve Clogged syringe Remove syringe and aspirate dispense liquid manually Clean syringe Bent needle Inspect and or change syringe No sample liquid is injected Check and or adjust Needle penetration into sample vial see chapter 4 2 Sample volume too low Mobile phase and or sample 77 The valve rotor is reversed 180 out of alignment flows out of the wrong ports on the LC injection valve Sample is backing up on the Syringe needle OD too small valve needle guide Increase sample volume Remove the rotor and reinstall in the correct position Look for a letter e g H stamped on the rotor The letter must be on the lower half of the rotor see chapter 13 3 Valve Rotor Check the syringe needle for gauge 22 Valve needle seal leaks Change Valve needle seal see chapter 9 2 Valve needle Guide The needle penetration depth for the injection valve is not set correctly Adjust the Injection Valve Needle Penetration see chapter 9 3 The Syringe Plunger Speed is too high resulting in excessive
66. th solvent from Wash2 SYRINGE Syringes Fill Speed Inject Speed Needle Penetr Clean Volume Max Fill Speed Max Eject Speed 23 Move to Home position 85 IFC PAL User Manual LC Inj Cycle Parameter Description Parameter biel SYRINGE Sample Volume Air Volume Pre Cln Slv1 Pre Cln Slv2 Pre Cln Spl Fill Speed Fill Strokes Pullup Del Inject to Inject Speed Pre Inj Del Pst Inj Del Pst Cln Slv1 Pst Cln Slv2 Viv Cln Slv1 Viv Cln Slv2 Description LC Inj Cycle Selected syringe Selected sample volume Volume aspirated after the syringe needle is moved out of the sample liquid Pre injection syringe wash strokes with solvent from Wash1 Pre injection syringe wash strokes with solvent from Wash2 Pre injection syringe rinse cycles with sample Speed of plunger movement used to aspirate sample Number of filling strokes to aspirate sample Delay time between sample pull up and ejection Name of Injector used for injection Speed of plunger movement used during sample injection Delay time prior sample injection Delay time after sample injection Post injection syringe wash strokes with solvent from Wash Post injection syringe wash strokes with solvent from Wash2 Valve rinse cycles with solvent from Wash Valve rinse cycles with solvent form Wash2 86 TO 5 Sam D A lt A UO li D HTS PAL Software Flow Chart 5puodas sajnu SINOH uiuo jo g LILONI Pok
67. the Parameter to be changed Assign the new value and press the ENTER key 3 Exit from Parameter List by pressing either the Home function key F4 to return to the top level Job Queue menu or the ESCape key to return to the previous menu 4 Method contents may be viewed from the Job Queue displays by selecting the desired Job pressing ENTER and the View Method function key 2 3 Delete Methods Methods can be deleted from the Method menu Methods in use by an active Job cannot be deleted Complete the following menu selections to delete a Method Menu Methods method name Del Method a el l IFC PAL User Manual Job and Job Queue Building and Starting a Job Queue Power up the IFC PAL The JOB QUEUE screen is displayed JOB QUEUE 03X Stkl Ol 001 096 eml 1 001 016 Method A Menuj Ada Del Start Job Job Figure 3 Example Job Queue Screen Load a sample Tray onto an available location in a Tray Holder or Stack Note the corresponding Tray name Add a new Job for the Tray Press the Add Job key to bring up the default Job For TRAY select the Tray Name e g Stk1 01 that corresponds to the location of the Tray that was just loaded Enter the First and Last sample number for this Job Select and enter the sample processing Method for this Job Press the Home function key F4 to return to the JOB QUEUE screen To add additional samples to be processed repeat steps 2 7 If necessary
68. tion Parameter may be changed by selecting the particular item Item Description Rinse Time Rinse Time may be used to expand the solvent flow time through the wash station glass liners after the last wash stroke is performed and the needle is retracted If Rinse Time is set to O the wash station valve is closed immediately after the last wash stroke 4 5 Dilutor The Dilutor functions are used for the Side port syringe from the IFC PAL Collector side By pressing a Function Key the following functions are available Function Key Description FI Prime This Function Is used to prime the solvent lines between the solvent bottle and the dilutor syringe and the transfer line between the dilutor syringe and the sideport syringe After selecting F1Prime the dilutor syringe aspirates the volume defined in Prime Volume and ejects the solvent to the selected Waste position It may be that several plunger strokes are needed depending on dilutor syringe size and Prime Volume The Function is used prior first time use or after every solvent or syringe change F2 Change The dilutor syringe plunger is moved to a position where the syringe can be removed DSyr from the dilutor module see page 9 assembling the PAL dilutor A prompt will be displayed to specify the new dilutor syringe The syringe must be installed before pressing Enter F3 Not used F4 HOME The dilutor syringe moves to it s Zero position and the Job Queue Menu is displaye
69. utl 3 the sample has been injected 4 Running Out Signal Active as long as the Job Queue is Off being processed and the PAL ts not in an error state 68 note l 11 1 IFC PAL User Manual PAL Loader Program The following procedures require a PC with Windows 95 98 NT 2000 XP Operating Svstem the supplied PAL Loader program Version 1 1 or higher the supplied grav cable Part RS9B 3000 and the correct version of the PAL firmware to be loaded Backing Up the PAL Control Program The following procedure should be performed after the installation of a new PAL System is completed Furthermore periodically System backups ensures that an updated configuration of the PAL is available any time Recommended practice is to create the following directory structure to store PAL firmware updates and backups Directory Path Contents C ProgramFiles PAL Loader Backup Full backup files of current and previous PAL configurations includes firmware and parameter settings maintained for archival purposes C ProgramFiles PAL Loader Update Extracted Update files in Loader format sss may include firmware only or firmware and parameter settings Shut off power to the PAL and the computer Connect the supplied gray cable between the PAL SER1 and a PC serial port Switch on power to the PAL When the PAL Job Menu is displayed start up the computer Double click the PAL Loader icon the PAL Loader screen appears EE lS
70. utton 7 Press Home The plunger moves down until it hits the mechanical stop This position is stored as the syringes zero volume position Then the Injection Unit returns to the HOME position Figure 32 Installing and Removing a Syringe from the PAL IFC Injector Side note After replacing a syringe always check the needle penetration in the LC valve see chapter 9 3 Injection Valve Needle Penetration 56 IFC PAL User Manual 8 4 Removing a Syringe Select Menu and press F1 Chang Syr The Injection Unit will move to a location that will facilitate removal of the syringe Loosen the plunger retaining screw Move the plunger slightly out of the plunger holder Pull the syringe adapter out and then carefully up to remove the syringe adapter with the syringe from the Injection Unit 5 IFC PAL User Manual 8 5 Installing a Sideport Syringe for the IFC PAL Collector Side 8 5 1 Installing the transfer tubing kit for IFC PAL Collector Side 1 Open the Torx screw at the guiding bracket of the sideport syringe adapter 2 Locate the transfer tubing kit end with 2 connection fittings 3 Insert the transfer tubing guiding wire into the guiding bracket slit 4 Adjust the guiding wire In a 90 angle to the bracket and tighten the Torx screw firmly Figure 33 Attaching the transfer tubing kit to the Sideport Syringe Adapter 58 IFC PAL User Manual 8 5 2 Installing the Sideport svringe for IFC PAL

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