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Chapter 4. Using the Endurance

1. 9910 2 Titerplate 96 127 75 40 25 Co o On x oO gt 4 o 03 5 9 Titerplate 384 Note The sides and ends will be straight within 0 50 mm This is defined as the maximum variation from a theoretical line connecting the applicable outside corners When the plate width is measured at its point of maximum deflection it will be as follows Length 127 75 384 titerplate or 127 5 96 titerplate 0 50 mm Width 85 5 0 50 mm 56 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Appendix C Error Codes The Endurance will display an error message if the user tries to enter invalid data Information on the allowed range will be displayed If something goes wrong in the physical operations of the Endurance an error code will be displayed Press the Start Stop key twice to lift the message and try to repair the failure condition with the help of the explanation of the code concerned Call your local service engineer if the problem persists Injection valve and ISS unit ERROR 11 ERROR 12 ERROR 13 ERROR 14 ERROR 15 ERROR 17 ERROR 18 Injection valve is not in a valid position The injection valve did not switch within 1 5 second
2. Figure 1 2 Back of the Endurance 1 2 3 4 5 6 7 8 9 SparkLink communication interface connector CE mark I O connectors Mains switch Mains input Fuses and voltage selector Type label Fan if plate cooling is installed Ventilation holes 0060 183 21 3 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 1 4 Keypad and display of the Endurance The keypad of the Endurance contains the following elements Soft function keys Cursor keys Stort Stop Numeric keys Holo Cont Methods Interrupt Menu Priority System Function keys Figure 1 3 Keypad and display Soft function keys the label assigned to these keys depends on the menu that is active The label of each key is shown in the bottom line of the display Cursor keys can be used to move to a different field in the display to move to a different field in a menu or to make a displayed value higher or lower Numeric keys e Oto 9 to enter numerals in the various programming fields e CL to clear a value in a field or replace it by NONE or AUTO e FE stands for Enter to go through menu lines or to confirm a choice made in a menu or a value entered The entered value is checked for validity and then saved Function keys e Run control keys Start Stop to start or stop automatic processing or to reset the system after an error
3. Replace plunger tip or Syringe Leaking Syringe Valve Replace Valve Rotor seal worn out Replace seal Check Stator N Redo connections with new Ferrules and nuts Dead volumes in tubing connections 82 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Appendix J Logbooks The following pages contain sample pages for logbooks that can be used with the Endurance Keep a record of settings System Menu and of programmed methods and templates Methods Menu for future reference Use copies of the provided pages 0060 183 21 83 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance User information Name of user Company Department Address Telephone Telefax Endurance information Serial number Firmware version Purchase date Installed options Local dealer Service engineer Address Telephone Telefax Comments 84 Artisan Technology Group Quality Instrumentation 0060 183 21 Guaranteed 888 88 SOURCE www artisantg com System Menu settings User manual Endurance lt GENERAL gt lt USAGE gt Loop volume UL Protection code Timebase methods enabled Needle tubing volume uL ldisabled Syringe volume uL Mix methods e
4. 8 Putthe new stator face assembly on the stator The three pins on the assembly fit the mating holes in the stator only one way 9 Mount the stator and stator face assembly on the valve so the stator locating pin in the stator ring enters the mating hole in the stator 10 Replace the three stator screws Tighten each an equal amount until the screws are tight at 4 l Stato Stator Suport Ring Stator Screus 3 Figure F 4 Exploded view of Model 9740 0060 183 21 69 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance F 3 Valco Cheminert Module C2 Valve Execute the following steps to clean and or replace the rotor Cleaning a valve can often be accomplished by flushing all lines with appropriate solvents Disassembly S See Figure F 5 exploded view 1 isolated to the valve Q Do not disassemble the valve unless system malfunction is definitely ROTOR Use a 9 16 hex driver to remove ie the socket head screws which secure the cap on the valve 2 To insure that the sealing surface of the cap is not damaged rest it on the outer face Or if the tubing is still connected leave it Figure F 5 Exploded view of the valve suspended by the tubing 3 With your fingers or small tool gently pry the rotor away from the driv
5. 888 88 SOURCE www artisantg com User manual Endurance 18 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Chapter 3 Getting started This chapter describes how to get started with the Endurance The following will be explained e menus of the Endurance e convenient working order e methods that can be programmed and linked to series e executing a series 3 1 Menus of the Endurance The software of the Endurance is menu driven The most important menus are e Ready Menu this menu appears after the Endurance has been switched on It offers very general possibilities for among other things methods management and communication with other apparatus e System Menu this menu appears after the System key in the keypad has been selected It offers general possibilities for entering settings for an analytical run Please note that settings may have been factory installed to suit particular wishes of the user In that case no changes will have to be made in the System Menu You are advised to enable only those facilities that you will need to ensure that other menus are as concise as possible e Methods Menu this menu appears after the Methods key in the keypad has been selected The menu allows you to program a method to be used in an analytical run and to assign a number to it e Series Menu this menu appears after the Series key in the
6. A rtisan Artisan Technology Group is your source for quality TecmoogyGroup new and certified used pre owned equipment FAST SHIPPING AND SERVICE CENTER REPAIRS WE BUY USED EQUIPMENT DELIVERY Experienced engineers and technicians on staff Sell your excess underutilized and idle used eguipment TENS OF THOUSANDS OF at our full service in house repair center We also offer credit for buy backs and trade ins IN STOCK ITEMS www artisantg com WeBuyEguipment Z EOUIPMENT DEMOS HUNDREDS OF InstraV ea REMOTE INSPECTION LOOKING FOR MORE INFORMATION MANUFACTURERS Remotely inspect equipment before purchasing with Visit us on the web at www artisantg com 7 for more our interactive website at www instraview com information on price guotations drivers technical LEASING MONTHLY specifications manuals and documentation RENTALS ITAR CERTIFIED i ki a k tia Contact us 888 88 SOURCE sales artisantg com www artisantg com ENDURANCE user manual Version 2 1 April 2000 0060 182 21 P O BOX 388 7800 AJ EMMEN THE NETHERLANDS TEL 31 591 631700 FAX 31 591 630035 E MAIL SALES SPARK NL Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com Artisan Technology Group Ouality Instrumentation Guaranteed 888 88 SOURCE www artisantg com CE DECLARATION OF
7. GE area Peak area ab n 1 Peak area RSD E x 100 Peak area 0060 183 21 61 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance E 1 3 Reproducibility test The default system settings were used except for the following lt GENERAL gt Air segment NO lt PLATES gt Location first transport vial 1 Location last transport vial 1 A deepwell plate is filled with sample on positions A1 A6 The transport solvent vial is filled with eluent The wash solvent bottle is filled with 80 H2O 20 Iso propanol Injection method Wash method Series Number 1 Number 1 Number 1 Type ul pick up Wash between injections First well A01 Analysis time 1 00 min Wash volume 300 uL Last well A 06 Injections well 3 Injection method 1 Injection volume 1 54yuL Wash method 1 Injection volume 2 Sul Injection volume 3 5 uL Example chromatogram of the reproducibility test 62 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com Peak Area number 1 206342 2 204773 3 205425 4 205203 5 205566 6 205568 7 206156 8 206174 9 205956 10 206165 11 205765 12 205960 13 206296 14 205617 15 205619 16 205648 17 206147 18 207070 User manual Endurance From the integration results the RSD for the Endurance can be calculated For this example the r
8. lt l0 gt lt CLOCK gt lt COMM gt Loopvolume Method protection Type of plate Inj Marker pulse System clock Device identifier Needle tubing code Process in ROWS Well marker pulse Date Syringe volume Use time base COLUMNS Lab Well marker Time O Syringe speed method Number of pulse Needle height Use mix method transport vials Input edge next inj Skip missing wells bd Use user program e Input edge next Air segment User program well e Headspace protection code e Freeze input active pressure e Use labeled wells e Reset outputs after Time base display Use templates series Key click Use calibration e Error buzzer wells Alarm buzzer Methods programming lt TEMPLATE gt lt METHOD gt lt USRPROG gt Userprog User program or ASPIRATE Mix method Methods DISPENSE Injection lt INJECTION gt lt WASH gt lt TIMEBASE gt lt MIX gt SYR VANE method SYRINGE Doo Injection methods Wash Timebase program Mix method MU meth lt FULL gt lt PARTIAL gt volume 4x AUX 1 ASPIRATE WAIT Wash 4x AUX 2 sample COMPRESS between 4x AUX 3 destination AUX Series 4x AUX 4 air Wells 4x ISS reagen WAIT INPUT Injections e 8xSSV e DISPENSE PROG OUT lt PICK UP gt e 8xCODE sample CODE OUT destination MARKERS e ENDTIME waste ssv reagen REPEAT WAI WASH Analysis time is ti Analysis time Flush volume Injection well Injection we
9. 100 E to define volume of 10 0 uL for 3rd injection Escape to return to the Methods Menu lt WASH gt to enter the Wash Menu 01 E to define wash method number 01 lt INJECTION gt E to select wash between injections 300 to define the wash volume Escape Escape to return to the Ready Menu 0060 183 21 25 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance To define the series Press keys Description Series to enter the Series Menu 01 E to define the series number 02 E to define the injection method for this series 01 E to define the wash method for this series lt ROW A gt 01 E to define the location of the first sample well lt ROW A gt 01 to define the location of the last sample well Escape to return to Ready Menu To run the series Put a vial with transport solvent mobile phase in transport vial position 1 left Make sure the transport vial is correctly filled before starting a new series Press keys Description Start Stop to start the Endurance 01 E to start at series 01 01 E to stop after series 01 lt START gt to start execution of the series At the end of the defined analysis time the Ready Menu will appear again to indicate that the Endurance is ready for the following next run 26 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOU
10. 74 75 77 alarm buzzer 34 analysis time 38 lt ASPIRATE gt 37 40 lt AUTOMATIC gt 33 lt AUX gt 39 41 B buffer tubing 1 2 11 13 buttons see keys c calibration wells 35 44 carry over test 63 65 CE mark 3 cL 4 19 lt CLOCK gt 36 lt CODE gt 39 41 lt COLUMNS gt 14 35 lt COMM gt 36 communication interface 3 lt COMPRES gt 41 condensed water and leakage 2 8 32 contact closures outputs 45 46 lt COOL gt 32 33 cooling 3 8 32 performance check 64 lt COPY gt 31 lt COUNT gt 32 cover 2 create template 30 cursor keys 4 19 D lt DATE TIME gt 33 lt DEFAULT gt 16 lt DEFAULT ALL gt 30 32 define series 24 26 29 30 lt DELETE gt 37 40 User manual Endurance lt DESTINATION gt 28 38 40 device identifier 36 lt DISPENSE gt 38 40 display 4 drain wash position 2 8 E E4 19 lt EDIT gt 37 40 lt END gt 39 lt ERASE gt 32 error beep 34 error codes 58 57 Escape 5 19 lt EVENTS gt 32 examples 23 30 lt EXCHANGE gt 14 15 31 lt EXIT gt 33 experienced users i extended needle 11 F factory installed items 52 fan 3 feeder option 15 17 first time users i first transport vial 35 fluid connections 1 flush volume 12 13 38 freeze input 47 48 freeze input active 36 full loop 1 11 13 73 75 fused silica needle 11 fuses 3 50 52 G lt GENERAL gt 33 34 Getting started 19 21 H headspace pressure 10 14 34 Help 5 lt HIGH gt 41 Hold Con
11. B Tronsporf Sample i Fluent Transport gt RSS DM MM i N gt pL pickup injections with A or without B air segment In case of uL pick up injections there will be no air pressure headspace pressure on the sample well to prevent errors due to air expansion during switching from sample well to transport vial You are advised to switch off use of an Air segment in the System Menu if the uL pick up injection method is used 78 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance I Trouble shooting Start up problems ee Power cord Plug in does not work m sle lt unplugged or Yes replace power after switching on 9 faulty cord of power S V N lt Blown fuse gt Yes gt Replace fuse w o oi p mi S Callyour ge Defective service electronics representative na pa S A Si Na The instrument is gt Display S Callyour working but service display doesn t lt component s gt i failure Z representative work ie Be ist A P NI f No response from Keyboard gt aa component s service keyboard but display works failure representative A Pa gt si Error code Check Appendix C appears on the p to locate error display message 0060 183 21 79 Artisan Technology Group
12. Connections The Endurance has six standard I O connectors on the rear side five OUTPUT connectors and one INPUT connector Refer to figure 1 2 for location of connectors The communication connector is a standard RS232 or an RS422 485 communication interface connector The configuration of the I O connector is described in the tables below The manufacturer will not accept any liability for damages directly or indirectly caused by connecting the Endurance to instruments CAUTION which do not meet relevant safety standards 6 1 Contact closures outputs The following three tables with programmable outputs P1 marker outputs P4 and auxiliary outputs P5 are contact closures outputs floating NO NC contact see figure 6 1 Table 6 1 Connector P1 OUTPUTS 2 programmable outputs and alarm output 1 OUT 1 Normally open 8 Spare 2 OUT 1 Common 9 Spare 3 OUT 1 Normally closed 10 Alarm output Normally open 4 OUT 2 Normally open 11 Alarm output Common 5 OUT 2 Common 12 Alarm output Normally closed 6 OUT 2 Normally closed 13 24 V DC 7 Spare 14 Power ground 15 Power ground Vax 28 Voc Vac Imax 0 25 A The Alarm output will be activated whenever an error occurs refer to Appendix C for a description of the error codes of the Endurance Table 6 2 Connector PA MARKERS 1 Inject marker Normally open 8 Labeled well marker Common 2 Inject marker Common 9 Labeled well marker Normally closed
13. and press E 6 Select the soft function key for the type of plate concerned 7 Press E and determine whether to process the plate in lt ROWS gt or lt COLUMNS gt 8 Press Escape twice to return to the Ready Menu A message appears to indicate that all programmed series will be reset The user will have to redefine series because the settings in the System Menu have been altered 14 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 2 9 Placing reagent vials transport vials Execute the following steps to replace reagent transport vials 1 Select soft function key lt EXCHANGE gt in the Ready Menu if Feeder option is installed select lt PLATES gt and select lt EXCHANGE gt The plate holder moves to the left 2 Take out the reagent vials transport vials figure 1 1 number 7 and replace them by other reagent vials transport vials 3 Select soft function key lt PLATE HOME gt The plate moves to operating position again Reagent and transport vials can be placed in any of the four positions Transport vials must be placed in a continuous row In the System Menu go to the Plates Menu to define the position for first and last Transport vial 2 10 Plate feeder The Plate feeder is a factory installed option that allows you to feed a maximum of 7 plates of the same type into the Endurance one plate on the plate holder and six in
14. and proceed Remove the three stator screws with the 9 16 hex key Remove the stator and stator ring from the valve body Pull the rotor seal off the pins Remove the isolation seal Mount the new isolation seal with the spring side facing away from the rotor seal Mount the new rotor seal The three pins on the shaft assembly fit into the mating holes in the rotor seal only one way Mount the seal with the grooves facing the stator 7 Replace the stator ring so that the body locating pin in the stator ring enters the mating hole in the body 8 Mount the stator on the valve so the stator locating pin in the stator ring enters the mating hole in the stator 9 Replace the three stator screws Tighten each an equal amount until the screws are tight ON o po Ni F 2 Operating Instructions for Rheodyne Model 9740 Valve Shaft Assembly Shaft Assembly Rotated Rotated Clockwise Counterclockwise Figure F 3 Flow diagram of model 9740 as viewed from stator Model 9740 is a two position six port PEEK valve Figure F 3 shows the flow diagram of the valve The six small circles represent the ports in the valve stator The slots are the connecting passages in the rotor seal Rotation of the valve 60 switches the valve from one position to another Specifications Maximum temperature is 50 C The valve is set to hold 345 bar 5000 psi The wetted surfaces are PEEK alumina ceramic and an inert polymer 68 0060 183 21
15. gt to define a pause H MM SS maximum of 9 hours 59 minutes and 59 seconds During the pause the needle will move to home position if the previous step is an aspirate or dispense action If you want the needle to stay in the same position an aspirate or dispense step of 0 uL must be programmed at the desired position lt REPEAT gt enter the number of steps that must be repeated and how often they must be repeated lt WASH gt enter the volume for needle wash Buffer is rinsed to waste lt INJECTION gt Use this key to program a method that defines injection methods max 24 for a run of the types full loop partial loopfill or uL pick up Enter a number for the injection method you are going to program If the selected method is locked because of changes in the settings System Menu after programming the method the word LOCK is displayed The method can be unlocked by programming valid values in the method itself or by restoring the values in the System Menu Use the soft function keys to select an injection method then enter values for analysis time the time between switching the injection valve to inject and the start of processing the next sample flush volume the amount of sample taken from a vial before the loop is filled with sample Default value 30 uL combined with an air segment Flush volumes of less than twice the volume of the needle and tubing will result in decreased performance number of injecti
16. guotations drivers technical LEASING MONTHLY specifications manuals and documentation RENTALS ITAR CERTIFIED i ki a k tia Contact us 888 88 SOURCE sales artisantg com www artisantg com
17. keypad has been selected The menu allows you to define a series and to assign a number and a method to it for the analytical run Use the following keys to go through the menus E ENTER to confirm a choice or to select a choice made in a screen or to step through menu lines cursor keys to change values in a field or to move to a different field in a screen Escape to return to a previous menu CL to remove a value from a field and enter NONE or DEFAULT soft function keys labels displayed in bottom line of the screen to go to submenus If MENU or MN is displayed in the top right hand corner of the screen you can press the Menu key in the keypad to display more possibilities offered by the menu Refer to section 1 4 for an explanation of all keys in the keypad 0060 183 21 19 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 3 2 Convenient working order After you have determined what type of analytical run you want to perform the most convenient working order for the Endurance is 1 Enter settings in the System Menu Note that the settings for the Endurance probably already have been correctly entered factory installed 2 Program a method for the analyses you wish to perform in the Methods Menu 3 Define a series and link a programmed method to a range of wells in the Series Menu 4 Execute the series Please note that it is allowed to
18. ports of the valves Press E to scroll through programming lines Only if SSV option is installed Enter the time and the SSV port number value between 1 and 6 Figure 5 1 ISS valve interconnected ports lt CODE gt lt END gt outputs enter a time and a value between1 and 15 hexadecimal output Press E to scroll through the programming lines to enter the end time for timed events program press E to scroll through the programming lines If no value is filled in or if CL is pressed the Endurance will automatically generate an end time The end time is equal to the analysis time programmed in the injection method used in the same series If end time exceeds the programmed analysis time this end time overrules the analysis time It is possible to program events after the end time but these events are not carried out during a run 0060 183 21 39 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance lt USER PROGRAM gt The user program offers the possibility to program all possible actions reguired for a sample handling seguence in separate steps Note that the total number of steps for the user program and all nine mix methods cannot exceed 240 The user program can be protected by a special user program protection code System Menu Usage Menu If no user program has been programmed yet end of user program is displayed Otherwise
19. separate injection methods 5 wash methods 5 timebase methods 9 mix methods and one user program It is also possible to program a combination of methods and save them in a template The settings entered in the System Menu determine the possibilities offered by the Methods Menu lt TEMPLATE gt Use this key to enter a menu in which the contents of a template can be defined First assign a number to the template then link the numbers of methods to the template The following items can be entered to fill a template e user program instead of methods if soft function key lt YES gt is selected the complete template is filled with the user program no other methods can be added If soft function key lt NO gt is selected the template can be filled with the following e mix method number injection method number wash method number timebase method number A maximum of 24 templates can be programmed lt METHODS gt Use this key to enter a menu in which methods can be defined lt MIX gt if enabled in System Menu Usage Menu Use this key to program a method that allows you to perform pre injection sample handling e g pre column derivatization dilution or adding of internal standard Nine mix methods can be programmed the maximum number of steps that can be programmed for the total of 9 mix methods and the user program is 240 Assign a number to the mix method The Mix Menu appears e lt EDIT gt an existing step or a new step
20. steps in this method A connection diagram is shown in figure 6 3 Table 6 6 Connector P6 INPUTS TTL 1 NEXT INJECTION INPUT 9 Signal ground 2 NEXT WELL INPUT 10 Signal ground 3 FREEZE INPUT 11 Signal ground 4 STOP I O 12 Signal ground 5 INPUT 1 13 Signal ground 6 INPUT 2 14 Signal ground 7 INPUT 3 15 Signal ground 8 INPUT 4 0060 183 21 47 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Next injection input This input will start the next injection sequence when the Endurance is started in remote control When the injection sequence is finished the Endurance will wait for the next input From the Ready Menu a NEXT INJECTION INPUT will start the last programmed series In this case the Endurance will not wait for the NEXT INJECTION INPUT before continuing with the next injection The Endurance will execute the complete RUN as if it was started with the Start Stop key Next well input With this input the Endurance will perform the next injection from the next well even if not all injections from that well in the programmed injection method have been executed Freeze input The Endurance will freeze the analysis time for the time this input is active If the FREEZE INPUT is activated while the analysis time is not running the Endurance will perform all programmed pre injection sample handling mix method and loading part of the
21. switching sequence for a partial loopfill injection is schematically shown in the following figures The first three steps are identical to those for Full loop injections see H 1 For partial loopfill injections the sample loop is filled by transporting the programmed injection volume into the sample loop The injection valve switches into the INJECT position The sample loop is now part of the HPLC mobile phase flow path the sample is transported to the column The am analysis time starts NANNI Sample z El The next injection seguence will start with a flush of 50 of the programmed flush volume in case an injection from the same vial and no wash routine is programmed Otherwise it will start with a flush of the programmed flush volume If the aspiration of sample for the next injection will exceed the total volume of the sample buffer tubing the buffer tubing is emptied before the next injection The next injection will start with the programmed flush see also the full loop injections 0060 183 21 75 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Air segment An air segment can be used to reduce the amount of flush volume This air segment is at the front of the flush volume and will not be injected Use of an air segment can be enabled in the System Menu General Menu Needle Inject
22. the feeder The following types of plates can be used with the feeder e 96 low plates max 6 plates in feeder e 96 high plates max 2 plates in feeder e 384 low plates max 6 plates in feeder The maximum height of plates that can be stacked into the feeder lift is 83 5 mm Q The 48 vials can not be used in the plate feeder Changes in operation if the Endurance Feeder option is installed e Inthe Series menu you have to enter a plate number to define the location of wells apart from the location of wells in rows and columns For example you can define the location of sample wells in a mix method on plate 1 and define the location of the destination wells on plate 5 e The Ready menu displays lt PLATES gt as the first soft function key press this key to enter the Direct control plate handling menu This menu offers the following possibilities lt EXCHANGE gt to move the plate holder Figure 1 1 number 9 lt LEFT LIFT gt to move the left lift up or down refer to Figure 2 4 lt RIGHT LIFT gt to move the right lift up or down refer to Figure 2 4 0060 183 21 15 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com Using the Feeder Make sure there are no plates in the left lift Define the type of plates you are going to use in the usual manner refer to section 2 8 Select lt PLATES gt in the Ready menu Select lt RIGHT LIFT gt in the Plates menu Sel
23. the first line of the programmed method appears The soft function keys appear e lt EDIT gt an existing step or program a new step for the user program e lt INSERT gt anew step before the displayed step e lt DELETE gt delete the displayed step The edit and insert menus offer the following soft function keys lt ASPIRATE gt a programmed volume from sample well ambient air destination vial wash or one of the reagent vials into the buffer tubing Speed and height of syringe can be entered refer to table 5 3 The maximum volume that can be aspirated is the total volume of the syringe lt DISPENSE gt a programmed volume from the buffer tubing into the sample well waste destination vial wash or one of the reagent vials Soeed and height of syringe can be entered refer to table 5 3 It is not possible to dispense a larger volume than the total volume aspirated in previous actions lt SYR_VALVE gt to control the connections of the syringe to one of its three tubes lt NEEDLE gt connection to sample needle lt WASH gt connection to wash solvent bottle lt WASTESs gt connection to syringe waste tubing lt SYR gt to control the movements of the syringe lt LOADs gt the syringe with the programmed volume lt UNLOAD gt the syringe with the programmed volume lt HOME gt the volume previously aspirated will be dispensed to the last programmed position and the syringe will be initialized again lt WASH gt t
24. waste and to move the syringe to standard operating position again lt UTILS gt Use this key to go to the Utilities Menu If use of a method protection code is enabled in the System Menu the code must be entered to access the Utilities Menu The menu offers the following possibilities 0060 183 21 31 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance lt COPY gt To copy a method Enter the type mix injection timebase wash and the number of the method to be copied Then enter a number to define the destination method Any existing method stored under that number will be overwritten lt ERASE gt To erase a method Template Methods User Program If Template and User Program are disabled in the System Menu the soft function keys for erasing a standard Method mix injection wash timebase appear Note that it is not possible to erase the user program if the protection code for the user program is enabled in the System Menu lt LOG gt the Endurance keeps a log of system relevant events lt EVENTS gt records error messages that have been generated and keeps count of actions of valves syringe and feeder movements lt COUNT gt A message appears after every 50 000 syringe actions and after every 200 000 syringe valve actions Lifetime of syringe valve maybe exceeded Check for possible leakage Syringe if you do not replace the
25. 0 uL UL Pick up 77 UL Volumes smaller than 5 uL may be injected but reproducibility and accuracy may not be lt 0 5 for partial loopfill or lt 1 for uL pick up In short loop lt 100 uL loop has to be filled three times loop 100 uL 499 uL loop has to be filled twice loop 500 uL loop has to be filled 1 5 times For volumes larger than 200 pL Use the 2000 uL buffer use the appropriate sample loop size and the appropriate syringe syringe volume gt 2 x injection volume Injection volumes larger than 500 uL are possible but the sample may contaminate the syringe Program sufficient wash after use Overview of appropriate buffer tubing for each type of syringe Syringe Buffer tubing 100 uL 500 uL 250 uL 500 uL 500 uL 2000 uL 1000 uL 2000 uL 10 mL 15 mL The 10 mL syringe and the 15 mL buffer tubing can only be used in combination with the User Program and not with the standard injection methods 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 2 8 Plates and sample handling The Endurance accommodates use of the following types of plates e 96 low wells e 96 high wells e 384 low wells e 48 vials A sensor figure 2 3 number 8 takes care of plate availability detection plate height detection and vial detection Because the Endurance uses headspace pressure during sample injec
26. 22 x 47 mm incl cap min 40 mm incl cap 5 1000 uL 0 5 mm With air needle dual needle action Missing plate amp height detection by vial sensor gt 5 cm sec Electrically lt 100 msec Built in compressor 250 mL internal wash solvent bottle 100 uL 250 uL standard 500 uL 1000 uL or 10 mL S316 PTFE TEFZEL VESPEL Glass Teflon Optional PEEK Fused silica Analytical performance Capped and sealed vials e full loop injections e partial loopfill injections e uL pick up injections Open vials plates valid at 1 0 cP e full loop injections e partial loopfill injections e uL pick up injections Memory effect Reproducibility RSD lt 0 3 RSD lt 0 5 injection volumes gt 5 uL with headspace pressure on the vial and 30 uL pre flush with air segment RSD lt 1 0 injection volumes gt 5 uL with headspace pressure on the vial Reproducibility RSD lt 0 3 RSD lt 0 5 injection volumes gt 5 uL without headspace pressure on the vial and 30 uL pre flush with air segment RSD lt 1 0 injection volumes gt 5 uL without headspace pressure on the vial lt 0 01 with programmable needle wash 0060 183 21 53 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Programming Injection methods Injection volume Injections per vial Analysis time Needle wash Priority sample Series Phys
27. 3 lnject marker Normally closed 10 STOP I O Normally open 4 Well marker Normally open 11 STOP I O Common 5 Well marker Common 12 STOP I O Normally closed 6 Well marker Normally closed 13 24 V DC 7 Labeled well marker Normally open 14 Power ground 15 Power ground Vax 28 Voc Vac Imax 0 25 A 0060 183 21 45 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Table 6 3 Connector P5 AUXILIARIES 1 AUX1 Normally open 8 AUX 3 Common 2 AUX 1 Common 9 AUX 3 Normally closed 3 AUX 1 Normally closed 10 AUX 4 Normally open 4 AUX 2 Normally open 11 AUX 4 Common 5 AUX 2 Common 12 AUX 4 Normally closed 6 AUX 2 Normally closed 13 24 V DC 7 AUX 3 Normally open 14 Power ground 15 Power ground Vmax 28 Voc Vac Imax 0 25A Q Maximum current for 24 Voc supply is 0 5 A total A Normally closed NC Common COM Normally open NO Figure 6 1 Contact closures outputs 6 2 TTL outputs The following tables show the marker outputs P2 and a 4 bit time base code output P3 programmable in a time base method Both connectors are TTL level outputs a connection diagram is shown in figure 6 2 Table 6 4 Connector P2 TTL OUTPUTS 1 INJECT MARKER 9 not connected 2 VIAL WELL MARKER 10 not connected 3 LABELED WELL MARKER 11 not connected 4 STOP I O 12 not connected 5 not connected 13 Signa
28. 70 ventilation holes 3 vials 14 53 voltage 52 voltage selector 3 WwW lt WAIT gt 38 41 lt WAIT IN gt 41 lt WASH gt 8 9 31 38 39 40 wash method 20 number 37 wash position 2 wash solvent 2 8 9 lt WASTE gt 28 40 waste tubing 8 well marker pulse length 36 well processing method 35 working order 20 96 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com 0060 183 21 Index of soft function keys lt ADJUST gt 16 lt ASPIRATE gt 37 40 lt AUTOMATIC gt 33 lt AUX gt 39 41 lt CLOCK gt 36 lt CODE gt 39 41 lt COLUMNS gt 14 35 lt COMM gt 36 lt COMPRES gt 41 lt COOL gt 32 33 lt COPY gt 31 lt COUNT gt 32 lt DATE TIME gt 32 lt DEFAULT gt 16 lt DEFAULT ALL gt 30 32 lt DELETE gt 37 40 lt DESTINATION gt 28 38 40 lt DISPENSE gt 38 40 lt EDIT gt 37 40 lt END gt 39 lt ERASE gt 32 lt EVENTS gt 32 lt EXCHANGE gt 14 15 31 lt EXIT gt 33 lt GENERAL gt 33 34 lt HIGH gt 41 lt HOME gt 40 lt INJECT gt 40 lt INJECTION gt 38 39 lt INSERT gt 37 40 lt lO gt 36 lt LEFT LIFT gt 15 31 lt LIFT DOWN gt 16 lt LIFT HOME gt 31 lt LIFT UP gt 16 lt LOAD gt 40 lt LOG gt 32 lt LOW gt 41 lt MANUAL gt 33 lt MARKERS gt 41 45 lt METHODS gt 37 42 lt MIX gt 37 38 lt NEEDLE gt 40 lt NEXT PLATE gt 16 lt PANIC gt 33 lt PLATE gt 16 lt PLATE HOME gt 14 15 31 lt PLATE
29. Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Use only plastic ferrules in the stator ports Metal ferrules can cause irreparable damage to the plastic stator CAUTION Maintenance With normal use the valve will give many tens of thousands of cycles without trouble The main cause of early failure which is seen as a leak in the valve is abrasive particles in the sample and or mobile phase which can scratch the rotor seal Following is the procedure for changing the rotor seal stator face assembly and isolation seal Refer to figure F 4 and proceed ng 1 Remove the three stator screws with a 9 64 inch hex I o aft sebi key pli Iwhttion Sal 2 Remove the stator stator face assembly and stator ring m m dy Location Pin from the valve body i i 3 Pull the rotor seal off the pins Stator Ring 4 Remove the isolation seal TJ Stator Location Pin 5 Mount the new isolation seal with the spring side facing i J H itr ate away from the rotor seal seily 6 Mount the new rotor seal The three pins on the shaft assembly fit into the mating holes in the rotor seal only one way Mount the seal with the grooves facing the stator 7 Replace the stator ring so that the body locating pin in the stator ring enters the mating hole in the body
30. CONFORMITY We Spark Holland BV Pieter de Keyserstraat 8 NL 7825 VE Emmen Declare that the product Autosampler Endurance types 920 921 is in conformity with the following documents e EEC directives 89 392 incl 91 368 and 93 44 machine safety and EEC directives 73 23 and 93 68 low voltage safety applied with the following standard EN 61010 1 Safety requirements for laboratory equipment Class I Installation cat Il Pollution degree II Spark Holland will not accept any liability for damages directly or indirectly caused by connecting this instrument to devices which do not meet relevant safety standards WARNING e EEC directives 89 336 and 92 31 EMC requirements applied with the following standards EN 50081 1 Generic emission standard EN 50082 1 Generic immunity standard EN 61000 3 2 Harmonic current emissions Use shielded cables and connectors for all remote connections Emmen November 14 1997 Rein van den Berg QA manager Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com Artisan Technology Group Ouality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance About this manual This manual has been written for laboratory technicians who use the Endurance for execution of analytical runs It is assumed that the user of this manual has basic knowledge of how to use menu driven software and that sh
31. ION 6 1 AT TIME 3 AUX 1 OFF AT TIME 3 ISS A POSITION 1 2 AT TIME 4 AUX 1 ON AT TIME 4 ISS A POSITION 6 1 AT TIME 4 AUX 1 OFF AT TIME 4 ISS A POSITION 1 2 AT TIME AUX 2 1 AUX 2 ON AT TIME SSV 1 SSV PORT AT TIME 1 AUX 2 OFF AT TIME 2 SSV PORT AT TIME 2 AUX 2 ON AT TIME 3 SSV PORT AT TIME 2 AUX 2 OFF AT TIME 4 SSV PORT AT TIME 3 AUX 2 ON AT TIME 5 SSV PORT AT TIME 3 AUX 2 OFF AT TIME 6 SSV PORT AT TIME 4 AUX 2 ON AT TIME 7 SSV PORT AT TIME 4 AUX 2 OFF AT TIME 8 SSV PORT AT TIME AUX 3 1 AUX 3 ON AT TIME CODE 1 CODE OUT AT TIME 1 AUX 3 OFF AT TIME 2 CODE OUT AT TIME 2 AUX 3 ON AT TIME 3 CODE OUT AT TIME 2 AUX 3 OFF AT TIME 4 CODE OUT AT TIME 3 AUX 3 ON AT TIME 5 CODE OUT AT TIME 3 AUX 3 OFF AT TIME 6 CODE OUT AT TIME 4 AUX 3 ON AT TIME 7 CODE OUT AT TIME 4 AUX 3 OFF AT TIME 8 CODE OUT AT TIME AUX 4 1 AUX 4 ON AT TIME 1 AUX 4 OFF AT TIME 2 AUX 4 ON AT TIME 3 AUX 4 OFF AT TIME 3 AUX 4 ON AT TIME 3 AUX 4 OFF AT TIME 4 AUX 4 ON AT TIME 4 AUX 4 OFF AT TIME END END OF TIMED EVENTS AT 0060 183 21 89 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Mix method Method number Line Action Value Position Sp
32. Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Analytical problems In case of analytical problems you will have to determine whether they are caused by the autosampler or by the rest of the system Quick check Replace the autosampler by a manual injection valve to discriminate between valve problems and other problems Perform a number of manual Full loop injections If the results are good the autosampler is faulty if not the HPLC system should be checked Syringe Valve k a Buffer tubing LE N a CG N A Ag k BIT Wa 74 lo V 4 Injection valve Needle arm Syringe 5 ii PR T needle se Mi Injection needle Z Hi In the flowcharts on the next pages it is assumed that the Endurance does not display any error messages Please keep in mind that analytical problems might be caused by external influences like temperature and or light sensitive samples For this reason it is important to make sure that the application was running without problems before and that no changes have been made in the settings System Menu 80 0060 183 21 Artis
33. Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Without Templates If you are going to execute an analytical run without using a template you will be asked to enter an injection method number and a wash method number and you will have to indicate the location of the first sample well and last sample well If you have enabled use of the calibration vial in the System Menu Usage Menu you will have to define whether you will use the calibration vial and indicate the number of wells between the calibration vial refer to figure 5 2 However if you have for example enabled use of a Mix Method in the System Menu Usage Menu you will also have to define the location of the First destination well and Reagent vials As soon as power is switched off all programmed series will be deleted It is not possible to leave the Series Menu before all values have been programmed Q Series are stored in the Endurance memory for as long as the power is on Calibration vials Sample vials OOO00OO0O O G OOOOOO dt L0OO _ gt _ 0 000 s 4 4 OOO OOOO OOO DO Figure 5 2 Injection sequence with 3 calibration wells between every 5 wells lt 4 44 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Chapter 6 I O
34. RCE www artisantg com User manual Endurance Example 3 A 1 10 dilution followed by a 10 pL partial loopfill injection This example describes how to let the Endurance transfer 360 uL from Reagent A to the destination vial add 40 uL of sample mix 3 times with 250 uL and subsequently inject 10 uL For system settings Press keys Description System to enter the System Menu lt USAGE gt E to enter the Usage Menu EE to go to the Mix field lt ENABLED gt to enable use of mix methods Escape to return to the System Menu lt PLATES gt E to enter the Plates Menu lt 96 HIGH gt to select 96 deepwell plate lt COLUMNS gt to select processing in columns A1 B1 etc CL to disable use of transport vials Escape Escape to return to the Ready Menu As soon as a change has been entered in the System settings the message ALL SERIES DEFAULT appears The user will have to redefine series because the settings have been changed To program the injection method Press keys Description Methods to enter the Methods Menu lt INJECTION gt 03 E to enter the Injection Menu lt PARTIAL gt E to select partial loopfill injection mode 100 E to define the analysis time 50 E to define the flush volume 3 E to define the number of injections per well 100 E to enter the injection volume for 1st injection 100 E to enter the injection volume for 2nd injection 100 E to enter the injection volume fo
35. S gt 2 14 35 lt PRIME gt 32 User manual Endurance lt PROG OUT gt 41 lt REMOTE gt 21 lt REPEAT gt 28 38 lt RIGHT LIFT gt 15 31 lt ROWS gt 14 35 lt SERIAL gt 33 lt SERVICE gt 33 lt SSV gt 32 39 41 lt START gt 21 24 lt SYR gt 40 lt SYR END gt 8 9 31 lt SYR HOME gt 8 9 31 lt SYR VALVE gt 40 lt TEMPLATE gt 30 37 lt TIMEBASE gt 39 lt UNLOAD gt 40 lt USAGE gt 35 lt USER PROGRAMS 40 42 lt UTILS gt 31 32 lt VALVES gt 39 40 lt WAIT gt 38 41 lt WAIT IN gt 41 lt WASH gt 8 9 31 38 39 40 lt WASTE gt 28 40 0060 183 21 Artisan Technology Group Quality Instrumentation 97 Guaranteed 888 88 SOURCE www artisantg com A rtisan Artisan Technology Group is your source for quality TecmoogyGroup new and certified used pre owned equipment FAST SHIPPING AND SERVICE CENTER REPAIRS WE BUY USED EQUIPMENT DELIVERY Experienced engineers and technicians on staff Sell your excess underutilized and idle used eguipment TENS OF THOUSANDS OF at our full service in house repair center We also offer credit for buy backs and trade ins IN STOCK ITEMS www artisantg com WeBuyEguipment Z EOUIPMENT DEMOS HUNDREDS OF InstraV ea REMOTE INSPECTION LOOKING FOR MORE INFORMATION MANUFACTURERS Remotely inspect equipment before purchasing with Visit us on the web at www artisantg com 7 for more our interactive website at www instraview com information on price
36. Signal ground Also indicated as GND in some devices 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 50 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Appendix A Installation The Endurance shipping container is supplied with a packing list Please check that all items mentioned in the list are included in the package before you start the installation procedure for the Endurance Do not install the Endurance in areas subject to shock dust or in direct sunlight Do not place it near a source of heat as this will disturb tray cooling if this option is installed The Endurance must only be connected to power sources and apparatus with protective grounding Execute the following steps to install the Endurance 1 Lift the Endurance from the shipping container Make sure you keep the apparatus upright lift it by placing your hands under the Endurance 2 Place the Endurance in its operating location preferably on the left hand side of the HPLC system Make sure the ventilation holes are not obstructed Allow the instrument to acclimatize for 1 hour 3 Install plate holder figure 1 1 number 5 in the Endurance on the flat surface underneath wash solvent bottle as far to the left and to the back as possible 4 Check whether local voltage m
37. acing 10 sample 10 standard 10 tubing 10 33 34 types 11 next injection input 21 47 48 lt NEXT PLATE gt 16 next well input 21 47 48 number of injections per vial 38 numeric keys 4 o options 55 59 P lt PANIC gt 33 partial loopfill 1 11 13 75 76 example 23 24 27 29 PC control 33 PEEK needle 11 Peltier cooling 3 8 32 33 performance Endurance 61 66 pictograms ii plate detection 10 14 plate feeder 15 17 plate holder 2 installation 51 lt PLATE gt 16 lt PLATE HOME gt 14 15 31 lt PLATES gt 2 14 35 94 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com in Ready Menu 15 17 31 51 types 35 56 preparations for use 7 17 lt PRIME gt 32 Priority 4 priority sample 4 5 lt PROG OUT gt 41 program method 24 25 27 28 programming keys 5 programming options 71 72 protection code 29 30 35 R r 21 Ready Menu 19 31 33 51 reagent vials 2 15 reference 31 44 lt REMOTE gt 21 remote control 21 47 lt REPEAT gt 28 38 replacement of parts 7 18 reproducibility 1 12 13 62 63 reset outputs after last series 36 lt RIGHT LIFT gt 15 16 31 lt ROWS gt 14 35 RS232 3 33 RS422 485 3 run control keys 4 run series 21 24 26 29 30 S sample handling 14 sample loop 11 13 sample loss 1 12 13 sampling needle 10 11 scale factor 33 34 42 lt SERIAL gt 33 Series 5 19 20 executing 21 in remote
38. alve to syringe valve PTFE tubing 640 mm x 146 O D x 1 0 mm I D volume 500 uL Tubing syringe valve to wash solvent bottle PTFE tubing 300 mm x 1 6 O D x 1 0 mm I D Tubing syringe valve to waste PTFE tubing 400 mm x O D x 1 6 mm I D For installation of HPLC connections waste tubing wash solvent syringe sample needle plates etc refer to Chapter 2 of this manual 52 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com Appendix B General Sound pressure level Working temperature Storage temperature Humidity Sample viscosity Safety Sample capacity Plates refer to figure B 1 Vial dimensions Reagent transport vials Loop volume Puncturing accuracy needle Pre puncturing septa caps Plate amp height detection Plate tray drive Switching time injection valve Headspace pressure Wash solvent Dispenser syringe Wetted parts User manual Endurance Specifications LeAq lt 70 dB 5 40 C 25 60 C 20 80 RH 0 1 5cP according to IEC 1010 1 plate 4 x 10 mL vials types 48 vials 96 low 96 high 384 low Max height vials 47 mm incl cap min height vials 12 5 mm incl cap Note Select high or low plates in System Menu Only plates of rigid material types can be used 6 x 8 vials dimensions base plate 128 x 85 8 mm Maximum outer diameter for each of 48 vials 12 mm Dimensions 10 mL vials
39. an Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance NO Blockage Disconnect INJECTION p P in Flow x needle from Path Valve Start _ Solvent a A manual P lt flowing out of gt Yes Check RI a V needle wash inj port n No Disconnect S Buffer tubing a from valve Stat lt Solvent gt manual gt lt out of open SS yes Check rotor zi seal wash end j Sg V NO Disconnect N VA Buffer tubing i from Syringe vae Start gt Solvent gt gt Check manual lt outof syringe gt Yesa buffer wash o valve lt tubing Y No ne v Leakage inside Injection Valve Disconnect the needle tubing and the buffer tubing Connect port 1 to an HPLC pump Block port 6 Start the pump at a low flow Check for over tightened connections in the entire Flow Path 8 Check the syringe valve a Pa i 4 e Pa Observe N ports3and4 gt Yes Check rotor ye seal for leakage i N S V Ss 4 Recheck with manual valve 0060 183 21 Artisan Technology Group Quality Instrumentation 81 Guaranteed 888 88 SOURCE www artisantg com User manual Endurance BAD REPRODUCIBILITY Air in Flow Path Start manual wash Leaking Syringe
40. ange Perform Move syringe Copy method Erase methods Logbook All methods Communication Prime solvent Service mode Lift_left standard wash amp Userprog erased all settings protocol valve Lift_right to default Plate System Settings System lt Menu gt lt GENERAL gt lt USAGE gt lt PLATES gt lt CLOCK gt lt COMM gt Loopvolume Method protection Type of plate Needle tubing code Process in Syringe volume Use time base ROWS Syringe speed method COLUMNS Needle height Use mix method Number of Input edge next inj Skip missing wells Use user program transport vials e Input edge next Air segment User program well Headspace protection code e Freeze input active pressure Use labeled wells e Reset outputs after Time base display Use templates series Key click Use calibration Error buzzer wells Alarm buzzer Inj Marker pulse System clock Device identifier e Well marker pulse e Date e Lab Well marker e Time pulse Methods Method lt INJECTION gt lt WASH gt lt TIMEBASE gt lt MIX gt Injection methods Wash Timebase program Mix method lt FULL gt lt PARTIAL gt lt PICK UP gt volume 4x AUX 1 Wash 4x AUX 2 between 4x AUX 3 Series 4x AUX 4 Wells 4x ISS ASPIRATE sample destination air reagent DISPENSE sample Analysis time Flush volume Injection well volume Inj volumes Injection well Inj volumes Injections 8
41. anual Endurance Vials ERROR 60 ERROR 62 ERROR 64 ERROR 65 ERROR 66 ERROR 67 ERROR 68 ERROR 69 Electronics ERROR 71 ERROR 72 ERROR 73 ERROR 75 Plate holder ERROR 90 ERROR 91 ERROR 92 ERROR 93 Plate feeder Missing vial Only available when Skip Missing Vial is set to NO in the System Settings and during the execution of the Mix of a sample on 48 vial plate Missing transport vial Missing vial for reagent A Missing vial for reagent B Missing vial for reagent C Missing vial for reagent D Missing destination vial Not enough transport liguid available due to missing transport vials Flexprint of the sample needle is not connected Invalid configuration of the Endurance PCB missing Current limit of the external I O exceeded Error occurred during initialization the Endurance cannot start Plate home time out plate did not reach home position home error Plate did not reach or leave home position during run Plate holder missing Dirt on the plate holder ERROR 80 Cannot rotate the grab head while needle is down ERROR 81 Grab head did not reach home position in time ERROR 82 Grab head not in home position when needle moving down ERROR 83 Grab head clamping timing error ERROR 94 Error grab head position ERROR 95 Left lift not empty before run ERROR 96 Horizontal or vertical position of grab head not reached in time ERROR 97 Lift home timeout 58 0060 183 21 Artisan Tech
42. atches voltage indicated on back panel of the Endurance 5 Connect the power cord to the Endurance figure 1 2 number 5 6 Switch the Endurance on by using the switch at the back of the apparatus figure 1 2 number 4 The Endurance now starts up The display indicates that a self test and initialization procedure are executed After completion of this procedure the following appears on the display 10 26 TUESDAY MAY 30 98 M READY x xx EXCHANGE gt lt WASH gt lt SYR END gt lt UTILS gt If the Feeder option is installed the following Ready menu appears 10 26 TUESDAY MAY 30 98 M READY x xx lt PLATES gt lt WASH gt lt SYR END gt lt UTILS gt 0060 183 21 51 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Factory installed items The Endurance is factory installed with e fuses in power switch 115 V AC 10 two 5 AT fuses slow 4x 14 UL CSA or 230 V AC 10 two 2 5 AT fuses slow 5 x 20 mm IEC127 100 uL loop 250 uL syringe 500 uL buffer tubing stainless steel 15 uL sample needle The fuses used are UL listed and CSA certified Tubing Material and dimensions Standard sample needle and tubing SS tubing 135 mm x 0 65 mm O D x 0 25 mm I D Tefzel tubing 140 mm x 6 O D x 0 25 mm I D total volume 15 uL Buffer tubing from high pressure v
43. control 21 Series Menu 19 42 44 parameters 43 without templates 43 44 with templates 43 44 lt SERVICE gt 33 settings see System Menu SILC needle 11 skip missing vials 34 soft function keys 4 User manual Endurance specifications 53 55 lt SSV gt 32 39 41 lt START gt 21 24 Start Stop 4 stop l O 47 48 symbols i ii lt SYR gt 40 lt SYR END gt 8 9 31 lt SYR HOME gt 8 9 31 syringe 2 9 11 13 replacing 9 types of 11 volume displacement check 65 waste 8 syringe speed 33 34 37 38 40 42 lt SYR VALVE gt 40 syringe volume 33 34 syringe waste tubing 2 System 5 19 System Menu 19 23 25 27 29 30 33 36 T Tefzel tubing 11 temperature control 32 33 lt TEMPLATE gt 30 37 template 20 create 30 example 29 30 enable disable 35 test procedure Endurance 61 66 lt TIMEBASE gt 39 timebase method 20 enable disable 35 number 37 time display 34 transport vials 2 15 35 trouble shooting 79 82 TTL inputs 47 48 TTL outputs 46 47 tubing 52 tubing holder 2 type label 3 typographical conventions i U lt UNLOAD gt 40 lt USAGE gt 35 lt USER PROGRAM gt 40 42 user program 12 13 20 21 33 0060 183 21 Artisan Technology Group Quality Instrumentation 95 Guaranteed 888 88 SOURCE www artisantg com User manual Endurance enable disable 35 user program instead of methods 37 using the Endurance 23 30 lt UTILS gt 31 32 V lt VALVES gt 39 40 valves 2 67
44. dard wash routine All tubing connected to the syringe valve is filled and rinsed Select the appropriate syringe in the System Menu and install the correct buffer tubing refer to section 2 7 go Figure 2 2 Replacing the syringe Note the 10 mL syringe can only be selected if the User Program is enabled in the System Menu Usage Menu 0060 183 21 9 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 2 5 Needle assembly The needle used for sampling consists of two parts prepuncturing needle a hollow needle used for puncturing of the septum capmat or sealer also used to put headspace pressure on the sample approximately 0 5 bar sample needle placed inside the hollow prepuncturing needle used for the actual transport of sample Different types of needles can be used here refer to section 2 6 and options mentioned in Appendix D If a needle with deviating diameter is used a different air outlet nut see figure 2 3 number 6 must be used that matches the injection needle Q Most commercially available sealers or capmats cannot be used in combination The following elements can be identified in the needle assembly Numbers 1 2 3 4 and 6 constitute the sample needle Execute the following steps to replace a needle 1 ON Oo BOM ZE with headspace pressure You are advised to switch off headspace pressu
45. durance To program a method Press keys Description Methods to enter the Methods Menu lt INJECTION gt 01 E program injection method number 1 lt PARTIAL gt E to select partial loopfill injection method 100 E to define an analysis time of 1 minute 030 E to define a flush volume of 30 uL 1 E to define the number of injections per well 100 E to set the injection volume at 10 0 uL Escape Escape to return to the Ready Menu To define the series Press keys Description Series to enter the Series Menu 01 E to define the Series number 01 E to define the injection method number CLE to enter lt NONE gt for wash method lt ROW A gt 01 E lt ROW A gt 01 E Escape to define location of the first sample well to define location of the last sample well to return to the Ready Menu To run the series Place a sample in position A 1 of the plate Press keys Description Start Stop to start the Endurance 01 E to start at series number 1 01 E to stop after execution of series number 1 lt START gt to start the analytical run The Endurance will now locate well A 01 and perform a 10 uL partial loopfill injection The display of the Endurance will indicate the status Checking tray Flushing Loopfill Running Rinse buffer Running The display also indicates the number of the defined series 01 the method number 01 and the well on which the analysi
46. durance Plate holder Plate holder for cool option Luerlock connection syringe valve Rheodyne loop 5 uL Rheodyne loop 10 uL Rheodyne loop 20 uL Rheodyne loop 100 uL Rheodyne loop 200 uL Rheodyne loop 500 uL Rheodyne loop 1000 uL Peek loop 20 uL Peek loop 100 uL Stator 7739 Rotor seal 7739 Tefzel rotor seal 7739 Peek stator 9740 Stator face assembly 9740 Peek rotor seal 9740 Wash solvent bottle 250 mL Syringe 1000 uL Syringe 10 mL Syringe100 uL Syringe 250 uL Syringe 500 uL 60 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Appendix E Test procedure The Endurance is factory tested for reproducibility carry over and mixing according to the following test procedure E 1 Analytical performance test E 1 1 Analytical system The Endurance is tested in an analytical system under the following conditions Pump flow 1 5 mL min eluent distilled water Detector wavelength 254 nm Sample Uracil in distilled water 50 ppm The following configuration was used PUMP 1 5 ml min UV Detector 254 nm me INtegrator 10 mtr SS tubing 0 25 mm ID for peak modelling E 1 2 Relative standard deviation RSD The following formulas are reguired for calculating the RSD x Peak area n
47. e Rheodyne Operating instructions Section F 3 below is a copy of Valco Technical Note 801 Valco Instrument Co Inc F 1 Operating Instructions for Rheodyne Model 7739 Valve Shaft Assembly Body Shaft Assembly Shaft Assembly Rotated Rotated Clockwise Counterclockwise Rotor Pins Figure F 1 Flow diagram of Model 7739 as viewed from stator Isolation Seal Model 7739 is a two position six port stainless steel valve Figure F 1 shows the flow diagram of the valve The six small circles represent the ports in the valve stator The slots are the connecting passages in the rotor seal Rotation of the valve 60 switches the valve from one position to another Rotor Seal Stator Ring Stator Location Pin Stator Specifications Maximum temperature is 100 C The valve is set to hold 345 bar 5000 psi The wetted surfaces are stainless steel and an inert polymer Stator Screws Figure F 2 Exploded view of model 7739 Maintenance With normal use the valve will give many tens of thousands of cycles without trouble The main cause of early failure which is seen as a leak in the valve is abrasive particles in the sample and or mobile phase which can scratch the rotor seal 0060 183 21 67 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Following is the procedure for changing the rotor seal and isolation seal Refer to figure F 2
48. e he is familiar with standard laboratory and HPLC terminology Chapters 1 and 2 of this manual contain basic information that should be read by every user of the Endurance e Chapter 1 identifies main parts of the Endurance e Chapter 2 explains how to install parts either for maintenance purposes or for preparing the Endurance for an analytical run For first time users e Chapter 3 explains the main menus of the Endurance and offers a basic explanation of how to operate the Endurance e Chapter 4 offers a number of examples that teach the user how to work with the Endurance For experienced users e Users who understand how the Endurance works will probably only use the reference part of this manual Chapter 5 to look up the purpose of a particular function e Experienced users may find the overview of programming options Appendix G useful for quick reference of possibilities of the Endurance The appendices in this manual offer specialist information An index has been provided to allow the user to find required information quickly Typographical conventions The following typographical conventions are used in this manual Initial Capitals are used for names of the menus Ready Menu Series Menu etc lt CAPITALS gt are used to refer to soft function keys bold type is used for names of keys in the keypad 0100 is used to indicate values that have to be entered with the numerical keypad Symbols The following symbo
49. e to a series a combination of various programmed methods mix injection wash timebase can be defined in a template The template is linked to a range of wells in a series In this way all steps in an analytical run are laid down and stored 20 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance e You can assign a user program to a series a possibility to combine all possible steps in the analytical process in one program The user determines the order of the separate actions the Endurance has to perform 3 4 Executing a Series Execution of a series is only possible if you have programmed a method and defined a series for the samples you wish to analyze Series are not stored in battery backup and exist only for as long as the Endurance is switched on Execute the following steps 1 Start programming the series by pressing Start Stop 2 Enter the number of the first series to perform and the number of the last series to perform 3 Select lt START gt to start the actual analytical run The Endurance starts to execute the series you have defined After the Endurance has executed the run the Ready Menu will appear again Refer to Chapter 4 for a number of examples illustrating this working order It is possible to program series and methods during a run Press Series or Methods the possibilities offered in the menus are identical to t
50. ect lt LIFT UP gt The lift moves up Place a plate on the right lift see Figure 2 4 number 2 Select lt NEXT PLATE gt to move the lift one position down You can now place another plate on the right lift Repeat step number 7 until MOM BR O Mo lt PLATE gt User manual Endurance To enter the plate height determination menu This menu offers the following possibilities lt DEFAULT gt For default plate sizes Height of one 96 low plate 14 5 mm Height of six stacked 96 low plates 77 mm Height of one 96 high plate 42 mm Height of two stacked 96 high plates 82 mm Height of one 384 low plate 14 5 mm Height of six stacked 384 low plates 79 mm lt ADJUST gt Before adjusting the plate height be sure the appropriate plate type has been selected in system settings System Menu Plates see section 2 8 The Adjust Menu allows you to calibrate the Endurance feeder to use plates of a different height 1 Place six or two plates depending on settings in the right lift refer to Figure 2 4 2 Place a ruler on top of the right lift 3 Select lt LIFT DOWN gt or lt LIFT UP gt until the top plate touches the ruler 4 Press E to confirm the height of the six stacked plates 5 Remove 5 plates from the right lift 6 Repeat steps 2 5 to calibrate the Endurance for single plate height 7 Press E to confirm the new plate height settings you have placed the reguired number of plates on the lift pre
51. eed Height Line Action Value Position Speed Height 1 41 2 42 3 43 4 44 5 45 6 46 Z 47 8 48 9 49 10 50 11 51 12 52 13 53 14 54 15 55 16 56 17 57 18 58 19 59 20 60 21 61 22 62 23 63 24 64 25 65 26 66 27 67 28 68 29 69 30 70 31 71 32 72 33 73 34 74 35 75 36 76 37 77 38 78 39 79 40 80 Comments 90 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User program User manual Endurance Line Action Value Position Speed Height Line Action Value Position Speed Height 1 41 2 42 3 43 4 44 5 45 6 46 7 47 8 48 9 49 10 50 11 51 12 52 13 53 14 54 15 55 16 56 17 57 18 58 19 59 20 60 21 61 22 62 23 63 24 64 25 65 26 66 27 67 28 68 29 69 30 70 31 71 32 69 33 73 34 74 35 75 36 76 37 77 38 78 39 79 40 80 Comments 0060 183 21 91 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 92 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com Index UL pick up 1 11 13 76 78 example 25 26 A accessories 57 58 accuracy 12 13 lt ADJUST gt 16 air outlet nut 10 11 air segment 34 73
52. eeeeeeceeeeeaeeeeeeeceeeeesaeeeeaaeeeeneeees 21 3 5 Executing a Series in remote control 21 Chapter 4 Using the Endurance ou ccccccecccsccesscsteseseetesesteseseeteseseene 23 Example 1 A 10 uL partial loopfill injection 23 Example 2 A 3 x 10 uL injection with UL pick up 25 Example 3 A 1 10 dilution followed by a 10 uL partial loopfill 27 Example 4 Defining a template and adding a protection code 29 Chapter 5 Reference eee 31 b l Ready Men sie aisicde ered dectesancteveedhecsepiadeds RAE 31 5 2 System MENU ccccceeececeeeceeeeeeeeeeceaeeeseaeseenaesseeeseaeeesaaeeteaeeeeees 33 5 3 Methods Menu ana 37 5 4 Series MENU sisri a aa aa R a aat 42 Chapter 6 I O Connections nnn 45 6 1 Contact closures outputS e 45 6 2 T TU OUUPUS ii iii korena aaea ie TEAR ENE AENT 46 6 3 TE PULS fancied cccsstacte ceanetevesinede ocsanenc esancadeceanetevesnieds dedna 47 6 4 MultiLink CONNECHOM eeeeeeeeeeeeeeeeeeeneeeeeeaeeeeeeaaeeeeeeaeeeeeenaeeeeneas 49 0060 183 21 v Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Appendix A Installation n 51 Appendix B Specifications 53 Appendix C Error codes an 57 Ap
53. ement tip 500 uL pck 10 0700 019 Plunger replacement kit 1 mL pck 10 0900 742 Plunger replacement tip 250 uL pck 10 0900 303 Sample needle including tubing ferrules and nuts 0900 304 Serum sample needle including tubing ferrules and nuts 0900 311 Peek sample needle including tubing ferrules and nuts 0900 318 Silica coated steel sample needle including tubing ferrules and nuts 0900 319 Silica coated steel serum sample needle including tubing ferrules and nuts 0900 321 Sample needle extra long including tubing ferrules and nuts 0060 183 21 59 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance number 0900 322 0900 323 0900 325 0900 326 0900 710 0900 711 0900 712 0900 713 0900 715 0900 718 0920 060 0920 315 0920 313 2140 160 3796 035 3796 009 3796 010 3796 012 3796 0131 3796 014 3796 015 3796 076 3796 016 3796 091 3796 092 3796 093 3796 095 3796 096 3796 097 4340 025 4400 000 4400 001 4400 030 4400 250 4400 500 description Serum sample needle extra long including tubing ferrules and nuts Peek sample needle extra long including tubing ferrules and nuts Fused silica needle including tubing ferrules and nuts Fused silica needle extra long including tubing ferrules and nuts Buffer tubing 500 uL Buffer tubing 2000 uL Syringe waste tubing Syringe wash tubing Buffer tubing 15 mL Air prepuncturing needle Shipkit En
54. ents Figure 1 1 Front view of the Endurance 1 Cover in open position 9 Plate holder 2 Buffer tubing 10 Drain wash position 3 Injection valve 11 Condensed water and leakage 4 Tubing holder 12 Wash position 5 Needle unit 13 Wash solvent bottle 6 Screw to fasten cover 14 Syringe 7 Transport reagent vials 15 Syringe waste tubing 8 Plate 2 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 1 2 Back view of the Endurance The back of the Endurance contains the following elements o o J opie ENE pe o o deno pa cee o O COMMUNCATION O SNET UUUULUULJUU uci ir AERO E o 2 e TEEN zs o o o RA ony 2 WARNING MAKE SIRE THAT AR OROJLATON UULUUHUUULDU WUL NOT BE INPEDED A a ee R o WARNING RISK OF FIRE REPLACE FUSE AS MED AVERTISSEVENT RISQUE DE FEU UU U U U U UU hia rise cowie noce se Ste see el o WARNING RISK OF ELECTRIC SHOCK DISCONNECT POWER BEFORE SERVICING U O U U U U U LJ Javertissement risoue DE cHoc ELecTRIQUE CE COUPER L ALIMENTATION AVANT LA MAINTENANCE o o o Pa MALNO amp MARKERS TTL
55. er 4 Examine the rotor sealing surface for scratches If scratches are visible to the naked eye the rotor must be replaced If no scratches are visible clean all the parts thoroughly with an appropriate solvent taking care that no surfaces get scratched The most common problem in HPLC is the formation of buffer crystals which are usually water soluble It is not necessary to dry the rotor Reassembly 1 Replace the rotor in the driver making sure that the rotor sealing surface with its engraved flow passages is facing out The pattern is asymmetrical to prevent improper placement 2 Replace the cap Insert the two socket head screws and tighten them gently until both are snug Do not over tighten them the screws simply hold the assembly together and do not affect sealing force which is automatically set as the screws close the cap against the valve body 3 Test the valve by pressurizing the system If it doesn t hold pressure the valve should be returned to Valco for repair 70 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Appendix G Programming options Ready Menu lt Menu gt lt EXCHANGE gt cwasH gt lt SYREND gt lt UTILS gt lt SERIAL gt lt SSV gt lt COOL gt lt SERVICE gt lt PLATES gt e Cool ON OFF lt COPY lt ERASE gt lt LOG gt lt DEFAULTALL gt Setpoint Switch ON OFF Exch
56. es are loaded in the loop e PEEK needle biocompatible needle e Fused silica needle needle with small inner diameter for small injection volumes e Extended needle needle for switching valve placed in the side panel of the Endurance e SILC needle needle for use with liquids that cannot be used with stainless steel needle Refer to Appendix D for an overview of options available for the Endurance Execute the following steps to install any of these needles 1 Remove needle as described in section 2 5 2 Remove the standard air outlet nut figure 2 3 number 6 and replace it by the nut supplied with the optional sample needle 3 Install optional sample needle as described in section 2 5 4 Adjust settings in System Menu General Menu to the volume of the new needle tubing see section 5 2 2 7 Combination of syringe sample loop and buffer tubing The 250 uL syringe is the standard syringe combined with the standard 500 uL buffer and the standard 100 uL sample loop the following injection volume range is available for the various injection modes Full loop 100 uL Partial loopfill 1 50 uL uL pick up 1 27 uL The maximum injection volumes are calculated with the following formulas Full loop injection volume loop volume Partial loopfill max injection volume 50 of loop volume uL pick up max injection volume loop volume 3 x needle tubing volume 2 0060 183 21 4 Artisan Technology Group Quality Instrume
57. esult is RSD z 0 25 The specified value is an RSD lt 1 E 1 4 Mixing and carry over test The default system settings were used except for the following lt USAGE gt Use of mix methods ENABLED A plate with one sample well filled with sample 50 ppm Uracil A01 one sample well filled with eluent A02 one empty destination A03 well and one Reagent A vial are placed in the Endurance A 1 10 dilution of sample from the sample well will be made in the empty destination well After dilution from both wells sample and destination 10 uL will be injected The Reagent A vial is filled with eluent The wash solvent bottle is filled with 80 H2O 20 Iso propanol 0060 183 21 63 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Injection method Series 1 Series 2 Number 1 Number 1 Number 2 Type partial loopfill Injection method 1 Injection method 1 Analysis time 1 00 min Wash method None Wash method none Flush volume 35 uL Mix method 1 Mix method none Injections well 3 First well A01 First well A01 Injection volume 1 10 uL Last well A01 Last well A 02 Injection volume 2 10 pL First destination well A 03 Injection volume 3 10 pL Reagent A vial 2 Mix method 1 Step Action Speed Height 1 Aspirate Sul Air 2 2 Aspirate 225 uL Reagent A 2 05 3 Dispense 180 uL to Destination 3 05 4 Dispense 50 uL to Waste 5 5 Repeat last 4 steps 1 time 6 Asp
58. for a new mix method e lt INSERT gt a new step in an existing method before the displayed step e lt DELETE gt the displayed step End of mix method means that the mix method is empty if an existing mix method is selected the first line of the mix method is displayed Scroll through the steps of the existing method with the cursor keys and use the soft function keys to enter changes in an existing method The following types of steps can be programmed for a mix method lt ASPIRATE gt sample air destination reagent A D a programmed volume Speed of syringe can be selected from 1 9 Refer to table 5 3 page 40 for values Height H indicated is the distance of the needle point to the plate holder default 5 mm The maximum amount which can be aspirated is the total volume of the syringe 0060 183 21 37 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance lt DISPENSE gt sample waste destination reagent A D a programmed volume from the buffer tubing Speed of the syringe can be selected from 1 9 Refer to table 5 3 page 40 Height H indicated is the distance of the needle point to the plateholder default 5 mm It is possible to dispense a larger volume than the volume aspirated in previous actions The aspirated amount will be complemented with liguid from the wash solvent bottle to total the programmed dispense volume lt WAIT
59. g com Injection methods User manual Endurance injection method number type full partial pick up Anal time Flush vol Inj per well Injection volumes 1 2 3 4 CO NI 4 BY Co N gt Comments 0060 183 21 87 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Wash methods Wash method Wash between Wash volume Comments number L linjections 1 L wells L series injections 2 L wells series injections 3 L wells series injections 4 L wells series L linjections 5 L wells series Comments 88 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com Timebase methods Method number User manual Endurance Action Time Action Time AUX 1 1 AUX 1 ON AT TIME ISS A 1 ISS A POSITION 6 1 AT TIME 1 AUX 1 OFF AT TIME 1 ISS A POSITION 1 2 AT TIME 2 AUX 1 ON AT TIME 2 ISS A POSITION 6 1 AT TIME 2 AUX 1 OFF AT TIME 2 ISS A POSITION 1 2 AT TIME 3 AUX 1 ON AT TIME 3 ISS A POSIT
60. ge volume these values have to be entered because the Endurance can be fitted with various types of syringes Every needle and needle tubing volume requires a different minimum flush volume The default flush volume equals two times the volume of needle and tubing The 10 mL syringe can only be selected if the use of the User Program is enabled in the System Menu Usage Menu When the 10 mL syringe is selected only the User Program can be used Use of other types of methods will be disabled e syringe speed and scale factor The aspirating speed of the syringe used in injection methods can be adapted depending on viscosity of samples Alternatively syringe 0060 183 21 33 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance speeds can be reduced by entering a scale factor The syringe speed will be the scale factor multiplied by the syringe speed The speed of the syringe during the wash or the rinsing procedure of the buffer are not affected by this setting See table 5 3 page 40 e needle height distance between the needle point and the plate holder default 5 mm The value is only used in injection methods for mix methods this value is programmable in the method itself e skip missing vials appears only if a plate with 48 vials is selected in System Menu Plates Menu YES means that empty spaces are skipped during the run NO means that the Endu
61. gs have been changed To select the methods to be incorporated in the template Press keys Description Methods to enter the Methods Menu 123456 E to enter the methods protection code lt TEMPLATE gt to enter the Template Menu 01 E to define the number for the template 02 E to define the injection method for this template 01 Escape Escape to define the wash method for this template to return to the Ready Menu To define the series Press keys Description Series to enter the Series Menu 01 E to define the Series number 01 E to define the Template method number lt ROW A gt 01 E lt ROW B gt 01 E Escape to define the first sample well to define the last sample well to return to the Ready Menu To run the series Press keys Description Start Stop to start the Endurance 01 E to start analysis at series 01 01 E to stop after analysis of series 01 lt START gt to start the analytical run The Endurance now performs the same actions as in Example 2 except that analysis is performed on two wells A 01 and B 01 Note select lt DEFAULT ALL gt in the Ready Menu Utilities Menu to erase all series and methods defined in these examples and to default all settings 30 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com 0060 183 21 User manual Endurance Chapter 5 Reference This c
62. hapter describes all possibilities offered by the Endurance software in the order in which they appear in the screen 5 1 Ready Menu The Ready Menu contains the following soft function keys lt EXCHANGE gt or lt PLATES gt if Feeder option is installed lt EXCHANGE gt Use this key to move the plate to the left in this position the plate can be replaced without damage to the eguipment Select soft function key lt HOME gt to move the plate to operating position again lt LIFT LEFT gt Use this key to move the lift up and remove the plates from the lift Select soft function key lt LIFT HOME gt to move the lift down again to operating position lt LIFT RIGHT gt Use this key to move the lift up and place plates on the lift Select soft function key lt LIFT HOME gt to move the lift down again to operating position lt PLATE gt Use this menu to calibrate the Endurance feeder to use plates of a different height refer to section 2 10 lt WASH gt Use this key to start a standard wash procedure All tubing connected to the syringe valve will be filled and rinsed with wash solvent lt SYR END gt Use this key to move the syringe to end position if you wish to replace the syringe needle or to simplify filling of wash solvent tubing A syringe volume of wash solvent is aspirated from the wash solvent bottle and the wash solvent tube is filled Select soft function key lt SYR HOME gt to dispense the syringe content to syringe
63. has occurred Hold Cont to hold or continue the analysis time The analysis time is extended by the period that Hold is active Interrupt not used Priority to stop a run to process a priority sample before analyzing the rest of the programmed sample series Before the run is interrupted processing of the present sample will be finished As soon as the priority sample has been analyzed the analytical run is resumed A priority sample is a series of one well with an injection 4 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance method a wash method and a time base method defined in a template only possible if the correct settings are entered in the System Menu e Programming keys see also section 3 1 and Chapter 5 Series to enter the Series Menu in which series can be defined for an analytical run Methods to enter the Methods Menu in which methods can be programmed for use in an analytical run Menu this key can only be used if MENU or MN is shown in the top right hand corner of the display Press this key to display more possibilities of the menu System to enter the System Menu in which system settings can be entered e General keys Escape allows the user to leave the programming mode or go to a previous level in the menu Entered values are checked for validity and then saved Help to display help information available only for a
64. he syringe dispenser aspirates the programmed flush volume from the sample well to fill the sample line with sample and remove wash solvents Sample hi The injection valve switches in LOAD position placing a sharp sample front at the inlet of the sample loop 0060 183 21 73 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance For full loop injections the sample loop is guantitatively filled by transporting two or more times the loop volume through the loop depending on the volume of the loop e loop lt 100 uL loop has to be filled three times e loop 100 uL 499 uL loop has to be filled twice e loop 500 uL loop has to be filled 1 5 times Sample URNIH The injection valve switches in INJECT position The sample loop is now part of the HPLC mobile phase flow A path sample is transported to the column The analysis Eine G3 SE a wam gt time starts Sample If one injection is to be done from each well or if a wash routine has to be performed after every injection the needle withdraws from the well directly after the injection and if programmed direcily performs a wash After the analysis time a new seguence is started If more than one injection is done from the same well without a wash routine the Endurance withdraws a flush volume after the analysis t
65. hose offered when the Endurance is idle If a series or method is changed the new values become active the next time the Endurance starts a series The series currently running are not affected by the changes 3 5 Executing a Series in remote control To execute a series from remote control execute the following steps 1 Press Start Stop 2 Enter the number of the first and the last series to be performed 3 Select lt REMOTE gt to enter the remote control mode The Endurance will now operate as slave of another device and can be controlled with Next injection input and Next well input To indicate that remote control is active an r is displayed in the bottom left corner of the display during execution of the series At the end of the series the message Series completed via remote control is displayed 4 Press Escape to return to the Ready Menu Refer to Chapter 6 for more information on remote control 0060 183 21 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 22 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Chapter 4 Using the Endurance This chapter describes a number of examples of actions that can be performed with the Endurance Please note that this chapter does not describe all types of actions that can be performed Try to do
66. ical Dimensions W x D x H with feeder option Weight with cooling option with feeder option with cooling and feeder Electrical Power requirements Fuses Communication OUTPUTS Full loop injections Partial loopfill injections UL pick up injections 5 uL 1 mL full loop depending on system settings 1 500 uL with 0 1 uL increments for partial loopfill 1 uL max volume with 0 1 uL increments for uL pick up max volume loop volume 3 x needle volume 2 Max 9 volumes are programmable for each injection Max 9 hrs 59 min 59 sec Programmable between injections wells or series Freely programmable Freely programmable 24 series max 280 mm x 400 mm x 440 mm 280 mm x 575 mm x 440 mm 23 kg 26 kg 29 kg 30 kg 115 VAC 15 20 50 Hz 60 Hz 250 VA 230 VAC 15 20 50 Hz 60 Hz 250 VA For 115 VAC two 5 0 AT fuses ax 1 UL CSA For 230 VAC two 2 5 AT fuses 5 x 20 mm IEC 127 All fuses UL listed and CSA certified Inject marker Well marker Labeled well marker Stop I O 4 Auxiliary outputs 2 Programmable outputs Alarm output 4 Bit timebase 54 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com INPUTS Serial Communication port PC control SparkLink Protocol Options Sample cooling Integrated stream switching ISS Solvent selection valve SVV Biocompatible option Biocompatible ISS valve Column o
67. ime to compensate for diffusion of mobile phase from the rotor groove into the first part of the sample line during the analysis time The flush volume between injections is not programmable and is always 50 of the programmed flush volume If the total amount of sample withdrawn with the next injection from the well will exceed the total volume of the buffer tubing the buffer tubing is emptied into the wash position before the next injection The next fill sequence will then start with a full flush volume Air segment An air segment can be used to reduce the amount of flush volume This air segment is at the front of the flush volume and will not be injected and therefore will not influence the injection Use of an air segment can be enabled in the System Menu General Menu With a standard needle the flush volumes must be minimal 30 uL for injections with air segment and 35 uL for injections without air segment If the samples are highly viscous it may be necessary to program larger flush volumes and reduce the syringe speed for better performance 74 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Needle njection loop Buffer tubing A Sample Fluent Flush Air o gt HL HL gt B i i Sample Eluent Flush gt Li Li gt A with air segment B without air segment H 2 Partial loopfill injections The
68. in 10 7 mL min 7 1370 L min 3430 uL min 6855 uL min 13710 uL min 13 7 mL min 8 1745 uL min 4365 uL min 8725 uL min 17450 uL min 17 5 mL min 9 2135 uL min 5335 uL min 10670 L min 21335 uL min 21 3 mL min During the dispense action the pressure in the buffer tubing will increase To prevent damage of the buffer tubing the flow should not exceed the value of caution 6 mL min for water Maximum speed 9 for 100 uL and 250 uL syringes speed 6 for a 500 uL syringe and speed 4 for 1000 uL and 10 mL syringe If more viscous liquids are used the speeds should be reduced 5 4 Series Menu This menu allows you to define the run sequence in a series A maximum of 24 series can be programmed A series contains information about the methods to be used for a range of wells This can be a template a separate method mix injection wash timebase or the user program Information on location of wells labeled wells or calibration wells is also programmed in a series If a feeder is installed you can define a plate number for each range of samples Q The settings entered in the System Menu and the methods defined in the Methods Menu determine which possibilities appear in the Series Menu 42 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Table 5 4 Series parameters Without templates With templates O Use user programYes No Template number Injec
69. injection method But the Endurance will wait with injecting the sample until the FREEZE INPUT is no longer active Stop I O With this input the run of the Endurance is immediately aborted The Ready Menu appears in the display In case the Endurance is in remote control the run of the Endurance is immediately aborted but the Endurance remains in remote control and cannot be restarted with a NEXT INJECTION INPUT INPUT 1 4 Programmable input can be used in the user program Active high Active low Autosampler Autosampler vec VCC z x O O Input s r Input s GND GND Figure 6 3 TTL input 48 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 6 4 Multilink connector The MultiLink connector is used to make the Triathlon communicate with the SparkLink software Set the dipswitch S1 and S2 as follows to let the ieee Si S2 communication work probably HO Gem Si 1 2 3 4 ON cel 88 26 a soj go NNNNO JE S2 1 2 3 4 OUT IN HE o Figure 6 4 MultiLink board m Mor Port Description S1 OUT to next device S2 IN to PC or previous device Connections for 9 pin connector TD Transmitted data to the computer pin 2 pin 3 RD Received data from the computer pin 5 SG
70. ion 2 10 are available for the Endurance These options enhance the uses for the Endurance considerably refer to Appendixes B and D for more information on options 1 1 Injection principle The Endurance offers three different methods of injection for an analytical run Full loop The sample loop is completely quantitatively filled with sample resulting in extremely good reproducibility Partial loopfill The sample loop is partially filled with sample this means low sample loss and programmable injection volumes UL pick up After aspiration of sample the sample is transported into the loop with transport liquid mobile phase this means no sample loss The Endurance uses a syringe to aspirate sample from a well into the sample loop To prevent contamination of the syringe the Endurance is equipped with a buffer tubing between the syringe and the injection valve Wash solvent is used to remove sample from the buffer tubing and sample needle and to rinse the buffer tubing and sample needle For more technical information on the injection principle used by the Endurance refer to Appendix H For an overview of fluid connections of the Endurance refer to the illustration inside the cover of the Endurance 0060 183 21 1 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 1 2 Front view of the Endurance The front of the Endurance contains the following elem
71. ion loop Buffer tubing Somple Eluent Flush Air gt LL Z 1 VV gt B 1 Seme Fluent Flush Wp A with air segment B without air segment H 3 uL pick up injections The switching sequence for a uL pick up injection is schematically shown in the following figures The initital situation the injection valve is in INJECT position The sample needle has entered the vial of transport liquid mobile phase to avoid disturbance of the chromatogram with an additional peak of the transport solvent after the air needle has prepunctured the septum The headspace pressure applied through the outer air needle ensures that no air or vapor bubbles are formed P E during wash solvent aspiration Transport liquid V 7 For the first injection after a wash or after emptying of the Si buffer tubing the syringe dispenser aspirates transport lt 5 Spgs tam liquid from the transport vial to fill the sample line with transport liquid and remove wash solvent Transport liquid 76 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance The needle moves from the transport vial to the sample well The injection valve is switched to the LOAD position lt a Syringe Column Needle Sample Transport liq
72. irate Sul Air 2 7 Aspirate 60 uL Sample 2 05 8 Dispense 40 uL to Destination 3 05 9 Dispense 50 uL to Waste 5 10 Aspirate 50 uL Air 2 11 Aspirate 200 uL from Destination 3 05 12 Dispense 200 uL to Destination 9 20 13 Repeat last 2 steps 3 times 14 End of mix method Example chromatogram of the mixing and carry over test 64 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Peak Area From the integration results the RSD for the two vials and the number carry over for the Endurance can be calculated 1 38802 2 38968 For this example the results are 3 39088 RSD well A01 sample 0 15 4 395258 RSD well A03 1 10 dilution 0 37 5 394090 6 394471 1 10 dilution lt 1 10 13 variation 1 29 7 The specified variation is 5 8 9 Carry over well A02 lt 0 2 No carry over detected in this test detection limit is 0 1 E 2 Syringe volume displacement check To check syringe volume displacement dispense a volume of 500 uL water from a sample vial to a destination vial with the following mix method Mix method 1 Step Action Speed Height 1 Aspirate 250 uL Sample 2 05 2 Dispense 200 uL to Destination 3 03 3 End of mix method Series 1 Number 1 Injection method None Wash method None Mix method 1 First well A 01 Last well A 01 First destination vial A 02 Reagent A vial 1 e Weigh the destinatio
73. l ground 6 not connected 14 Signal ground 7 not connected 15 Signal ground 8 not connected All markers are active low logical 0 Vmax 5 5 V logical 1 gt 3 5 V logical 0 lt 1 0 V DC output source sink current 20 mA A marker output pulse will be generated when the injection valve switches from LOAD to INJECT However in a User Program markers have to be programmed by the user 46 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Table 6 5 Connector P3 TIMED OUTPUTS 4 bit time base code output 1 oR WP TB 0 HEX TB 1 HEX TB 2 HEX TB 3 HEX not used 1 2 4 8 6 Signal ground 7 Signal ground 8 Signal ground 9 Signal ground Vmax 5 5 V logical 1 gt 3 5 V logical 0 lt 1 0 V DC output source sink current 20 mA Figure 6 2 TTL output 6 3 Autosampler Ext device K Output J Input TTL K GND GND TTL inputs The following connector is an active high or active low TTL input it can be defined in the System Menu The NEXT INJECTION INPUT and the NEXT WELL INPUT can be used when the Endurance works in REMOTE CONTROL The FREEZE INPUT and STOP I O input can be used to control the Endurance by other devices The four inputs INPUT 1 to 4 can only be used in the user program e g to control the seguence of the
74. limited number of functions 0060 183 21 5 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 6 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Chapter 2 Preparations for use This chapter describes procedures for replacement or installation of parts either for maintenance or for preparation of the Endurance for an analytical run Please note that the power should not be switched off for any of the procedures described below A number of items reguired for use of the Endurance are factory installed see Appendix A However after the installation procedure described in Appendix A has been executed check that the following have been correctly installed before you start to use the Endurance e HPLC pump 8 column connections e waste tubing e wash solvent bottle e syringe e needle assembly e syringe sample loop and buffer tubing e plate holder and plate e reagent vials transport vials e plates in plate feeder if feeder option is installed Loosen the screw at the right hand side of the cover figure 1 1 number 6 and lift the cover to execute the procedures described in this chapter 2 1 HPLC connections Make the following connections e HPLC pump to port 1 of the injection valve e HPLC column to port 6 of the injection valve The instru
75. ll Inj volumes Inj volumes With templates Without templates Series Template Userprogram yes no Use cal Nr 4 yes no or calibration interval Mix method Plate number Injection method Sample wells Wash method Destination wells Timebase method Note Reagent vials e Use cal wells yes no e Labeledwells calibration wells These parameters depend on the content of the calibration interval methods used and or the System Settings of the Plate number Endurance Sample wells Destination wells Reagent vials Note Labeled wells Optional Soft function keys Start Stop First series Last series Res E SSTARTO lt REMOTES Note only if Feeder option is installed 72 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Appendix H Injection principle This appendix offers specialist information on the injection principles used by the Endurance H 1 Full loop injections The switching sequence for a full loop injection is schematically shown in the following figures The initial situation the injector is in the INJECT position The sample needle has entered the well after the air neede has prepunctured the septum Headspace pressure is applied through the outer air needle to ensure that no air or vapor bubbles are formed during sample aspiration lt Syringe Colunn T
76. loop content when switching from inject to load position prior to sample loading Specially when working with high pressure 200 bar this loss may be 0 1 0 5 uL for a 100 uL loop Note that the minimum sample loss in partial loopfill mode is 30 uL recommended minimum flush volume for the first injection and an additional 15 uL always half the programmed flush volume for additional injections from the same well If a wash between injections has been programmed sample loss is 30 uL for every injection For zero sample loss injections use the uL pick up injection mode e uL Pick up use a 100 uL syringe for optimum accuracy and reproducibility Do not use a smaller sample loop The sample plug is transported into the loop preceded by a programmable air segment of 5 uL if selected in System Menu you are advised to switch off the air segment with uL pick up with a plug of transport liquid which equals 2 5 times the programmed needle tubing volume 12 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Injection volumes up to twice the standard With the standard 250 uL syringe standard needle with tubing 15 uL and standard 500 uL buffer but with a 200 uL sample loop the maximum injection volumes are Full loop 200 uL sample loss remains 230 uL since loops gt 100 uL need only one loop volume overfill 30 uL pre flush Partial loopfill 10
77. ls are used on the Endurance WARNING This sticker indicates that care should be taken to prevent N personal injury or damage to parts of the Endurance SHARP NEEDLE AND MOVING PARTS KEEP HANDS CLEAR 0060 183 21 i Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance gt This sticker with yellow background color at the back of the Endurance calls attention to the fact that you are expected to consult this manual for instructions on how to operate the Endurance The following pictograms are used in this manual gt D WARNING gt CAUTION calls attention to a procedure which if not correctly executed could result in injury or loss of life Do not proceed beyond a DANGER sign until the indicated conditions are fully understood and met calls attention to a procedure which if not correctly executed could result in personal injury Do not proceed beyond a WARNING sign until the indicated conditions are fully understood and met calls attention to a procedure which if not correctly executed could result in damage to the equipment Do not proceed beyond a CAUTION sign until the indicated conditions are fully understood and met calls attention to important information Read this information before continuing Safety practices The following safety practices are intended to ensure the safe operation of
78. m templates Pogram templates in the Methods Menu Default disabled e calibration wells to enable or disable the possibility of programming a calibration vial Program the the calibration vial in the Series Menu Default disabled You are advised to disable as many functions in the Usage Menu as possible to make sure that other menus do not contain possibilities that are irrelevant for the type of analyses you are to perform lt PLATES gt Use this key to define the type of plates that will be used Four types can be selected 96 low default 96 high 384 low or 48 vials After a plate type has been selected enter e well processing method in rows left to right or in columns top to bottom e first transport vial enter a number 1 4 or press CL last transport vial enter a number 1 4 Vials can be placed in any of the four positions Transport vials must be placed in a continuous row 0060 183 21 35 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance lt IO gt Use this key to enter the I O configuration mode and define the following e inject marker pulse length to define the length of the inject marker pulse e well marker pulse length to define the length of the well marker pulse e labeled well marker pulse length to define the length of the well marker pulse of the labeled well e input edge next injection to define
79. ment has been flushed with isopropanol before dispatch from the factory Make sure that the mobile phase of your HPLC system is miscible with isopropanol or start up with an intermediate solvent as mobile phase disconnect the HPLC column It is very important that the content of the sample loop is injected in back flush onto the column therefore do not exchange column and pump connections at the injection valve 0060 183 21 7 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 2 2 Waste tubing Make the following connections Syringe waste put the end of the syringe waste tube see figure 1 1 number 15 ina bottle placed next to the Endurance Drain wash position connect the hose to the drain wash connector of the Endurance see figure 1 1 number 10 place the other end of the hose in a bottle placed on the floor Through this drain all liguid dispensed to waste at the back of the plate is removed Condensed water and leakage connect the hose to the drain port of the Endurance see figure 1 1 number 11 Place the other end of the hose in a waste container on the floor Through this hose all leakage solvents and condensed water if Peltier cooling is installed are drained Make sure that the flow path of the hoses is not obstructed in any way 2 3 The Wash solvent Endurance has a 250 mL wash solvent bottle Execute the following steps
80. mix method step number 5 to repeat last four steps once to define mix method step number 6 to aspirate an air segment of 5 0 uL to define mix method step number 7 to aspirate 60 0 uL of sample to define mix method step number 8 to dispense 40 0 uL to destination well to define mix method step number 9 to dispense 50 0 uL to waste to define mix method step number 10 to aspirate an air segment of 50 0 uL to define mix method step number 11 to aspirate 200 0 uL from the destination well to define mix method step number 12 to dispense 200 0 uL to the destination well to define mix method step number 13 to repeat the last 2 steps three times to return to the Ready Menu 28 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com 0060 183 21 To define the series User manual Endurance Press keys Description Series to enter the Series Menu 01 E to define series number 1 01 E to select Mix method number 1 for this series 03 E to select Injection method number 3 CLE to select lt NONE gt for wash method lt ROW A gt 1 E to define location of first sample well lt ROW A gt 1 E to define location of last sample well lt ROW B gt 1 E to define location of first destination well 1 E to define position of Reagent A Escape to return to the Ready Menu To run the series Put sample in position A 01 position B 01 is used as empty desti
81. n vial before and after the Run e The difference is the aspirated volume e The specified variation is 2 0060 183 21 65 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance E 3 m ON s Tray cooling performance check Place a thermocouple on the bottom of the tray make sure the contact is good Switch on the tray cooling and program a setpoint of 10 C Wait minimal 15 minutes for equilibration of the Endurance Read out the temperature of the thermocouple The value must be in a range of 2 C of the programmed setpoint E 4 NO mamo M Loop performance check Disconnect the loop from the injection valve Remove all liguids from the loop with air Weight the empty loop on an analytical balance Fill the loop with minimal 2 times its volume of water Weight the filled loop again The difference is the weight of the capacity of the loop The weight divided by the specific weight of water 1 g mL gives the volume of the loop Allowed variation 10 66 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Appendix F Injection valves The Endurance can be equipped with the following injection valves e Rheodyne 7739 valve e NRheodyne 9740 valve biocompatible e Valco Cheminert Module C2 valve Sections F 1 and F 2 below are a copy of th
82. nabled disabled Syringe speed factor User program lenabled Needle height mm disabled Skip missing vials lyes Jno User program protection code Air segment Llyes Jno Labeled wells lenabled Headspace pressure Llyes Jno disabled Time display HH MM SS H MM mm Templates LJenabled disabled Key click Jon off Error beep lon Loff Calibration wells Jenabled Alarm buzzer lon off disabled lt PLATES gt lt lO gt _ 96 low Inject marker pulse length S C 96 high 384 low Well marker pulse length SEC 148 vials Labeled well marker pulse processing in length SEC ROWS L COLUMNS Input edge next injection L falling L Jrising position first transport vial Input edge next well L falling L rising position last transport vial Freeze input active L low Jhigh Reset outputs after last series yes Cno lt CLOCK gt lt COMM gt JOn yy mm dd and hh mm Device identifier 2 Off Comments 0060 183 21 85 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Templates Template Injection Mix Wash Timebase User program Comments number method method method method Y N Comments 86 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisant
83. nation well Place a filled reagent vial in position 1 Make sure the reagent vial is filled correctly before starting a new series Press keys Description Start Stop to start the Endurance 01 E to start at series number 1 01 E to stop after series number 1 lt START gt to start processing of sample The Endurance will now start searching for the Reagent vial and transport 180 uL to the destination well twice then 40 uL of sample will be added and after mixing 3 times a 10 uL injection will be performed Example 4 Defining a template and adding a protection code This examples describes how to incorporate the injection method 02 and wash method 01 defined in example 2 in a template A protection code will be added For system settings Press keys Description System to enter the System Menu lt USAGE gt E to enter the Usage Menu 123456 E to enter a 6 digit code memorize this code 0060 183 21 29 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance E lt DISABLED gt E EE lt ENABLED gt Escape Escape to go to the mix methods field to disable use of mix methods to go to the template field to enable templates to return to the Ready Menu After use of templates has been enabled the message ALL SERIES DEFAULT appears The user will have to redefine series because the settin
84. nction keys can be selected 32 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance lt MANUAL gt temperature control will remain ON until it is switched off again by the user in this menu lt AUTOMATIC gt temperature control will be switched OFF after all programmed series have been executed lt DATE TIME gt temperature control will be switched ON or OFF depending on initial situation at a date and time that can be programmed lt SERIAL gt Use this key to put the Endurance in serial mode to allow for control of the autosampler by way of PC RS232 interface Select a device identifier in the System Menu refer to section 5 2 If a method protection code was defined in the system settings this code must be entered to get access to serial mode The following soft function keys appear lt PANIC gt press this key to begin a stop sequence in which all tubing is rinsed and the valve and I O ports are reset At the end of the sequence serial mode is resumed lt EXIT gt press this key to end serial mode and return to the Ready Menu lt SERVICE gt For service to the apparatus To be used by authorized personnel only The Service Menu is protected by a service code 5 2 System Menu The System Menu contains the following soft function keys lt GENERAL gt Press this key to enter values for e loop volume needle tubing syrin
85. needle wash routine if a needle wash is used to control the four standard auxiliaries contact closures Refer to Chapter 6 to program a pause in which the Endurance waits for one of the four inputs to become lt HIGH gt or lt LOW gt before continuing with the next step Refer to Chapter 6 to define two programmable outputs contact closures These are similar to the auxiliaries but only available in the user program Refer to Chapter 6 to program the output to the connector P3 TIMED OUTPUTS This is a HEX output in the range 0 to 15 Refer to Chapter 6 the markers normally generated in the Endurance are not active in the user program but can be programmed in this screen refer to Chapter 6 Select marker and status inject vial labeled option to define the Solvent Selection Valve SSV port position range 1 to 6 0060 183 21 41 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Table 5 3 Syringe speed SYRINGE 100 pL 250 uL 500 pL 1000 uL 10 mL SPEED 1 50 uL min 125 uL min 250 uL min 500 uL min 0 5 mL min 2 low 125 uL min 315 uL min 630 uL min 1255 L min 1 3 ml min 3 normal 250 uL min 625 uL min 1250 uL min 2495 uL min 2 5 mL min 4 high 375 uL min 940 uL min 1880 uL min 3765 uL min 3 8 mL min 5 770 L min 1920 uL min 3840 uL min 7680 uL min 7 7 mL min 6 1070 uL min 2675 uL min 5335 uL min 10665 L m
86. nged end for valve fitting and place a larger bottle next to the Endurance To fill the wash solvent tube you may have to repeat the above mentioned filling procedure steps 6 and 7 a few times 2 4 Syringe The Endurance is supplied with a 250 uL syringe It is also possible to use the Endurance with a 100uL 500 uL 1000 uL or 10 mL syringe Execute the following steps to install a syringe 1 Select soft function key lt SYR END gt in the Ready Menu to w S move the syringe to end position we A 2 Lift the cover Unscrew the top of the syringe turn clockwise 4 Pull the bottom of the syringe towards you you can now Re remove the syringe refer to figure 2 2 5 Fill the new syringe with wash solvent and make sure that all air bubbles are removed from the syringe 6 Connect the bottom of the filled syringe to the Endurance 7 Screw the top of the filled syringe to the Endurance counter clockwise 8 Lower the cover 9 Select soft function key lt SYR HOME gt to remove air from gt the syringe The syringe moves to home position and its h content is dispensed to waste s 10 If any air remains in the syringe select lt SYR END gt again to fill the syringe with wash solvent press lt SYR HOME gt again to move content to waste Repeat if there is still air in the syringe and gently tap the syringe as wash solvent is dispensed to waste 11 Select soft function key lt WASH gt in the Ready Menu to execute a stan
87. nology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Appendix D Options and accessories The following configuration options are available for the Endurance number SP920 002 SP920 010 SP920 012 SP920 020 SP920 030 0900 837 SP880 050 SP880 051 0920 852 description Endurance Bio Autosampler with inert injection valve and sample needle Endurance ISS Autosampler with one Integrated Stream Switching valve Endurance Bio amp ISS Autosampler with inert injection valve and inert ISS option Endurance SSV Autosampler with Solvent Selector Valve SSV for multiple solvents Endurance SSV amp ISS Autosampler with SSV and ISS option Injection valve mounted on right side of Endurance Mistral slave HPLC column thermostat to be used in combination with Endurance autosampler Mistral cool slave Peltier cooled HPLC column thermostat to be used in combination with Endurance autosampler Plate feeder for maximum 6 low plates The following accessories are available for the Endurance number description 0043 364 Needle wash insert vial 0043 473 Needle body 0700 002 Long Bushing Rheodyne pck 10 0700 003 Ferrule Rheodyne pck 10 0700 008 Rheflex ferrule pck 10 0700 009 Rheflex nut pck 10 0700 010 Flanged tube fitting 1 8 pck 5 0700 011 Flanged tube fitting 1 16 pck 5 0700 012 Plunger replacement tip 100 uL pck 10 0700 018 Plunger replac
88. ntation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Five sizes of syringes can be used in the Endurance 100 250 500 1000 uL and 10 mL The 10 mL syringe can only be used in the User Program must be enabled in System Menu see section 5 3 and not for the standard injection modes Full loop gives maximum reproducibility RSD lt 0 3 but not maximum O accuracy since loop volume is specified with an accuracy of 10 Minimum sample loss 230 uL 2 x loop overfill flush volume for needle for the standard 100 uL loop Partial loopfill gives maximum accuracy depends on syringe accuracy and reproducibility better than 0 5 RSD for injection volumes gt 5 uL Minimum sample loss Flush volume 30 uL 30 uL is the recommended minimum flush volume combined with an air segment smaller flush volumes can be programmed but will result in decreased performance pL Pick up means zero sample loss maximum accuracy same as partial loopfill but slightly diminished reproducibility RSD better than 1 for injection volumes gt 5 uL If an air segment is selected in the System Menu 5 uL of air is injected together with the sample For some cases other combinations of syringe loop and or buffer are advised Injection volumes smaller than 5 pL e Partial loopfill use a 100 uL syringe for maximum reproducibility and accuracy Use a 20 uL sample loop to avoid loss of accuracy due to expansion of the
89. o execute a needle wash the content of the buffer tubing is not rinsed to waste before the start of the wash The programmed volume of wash solvent is used to wash the needle at the wash position tubing which may generate cross contamination To prevent contamination of the wash position program a dispense to waste action before programming a wash action Q The wash position may be contaminated with the contents of the buffer lt VALVES gt to program positions of high pressure valves ISS injector valve SSV The injector valve has two positions lt INJECT gt and lt LOAD gt The ISS optionional valve has positions 1 6 and 1 2 see figure 5 1 40 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com lt WAIT gt lt COMPRES gt lt AUX gt lt WAIT IN gt lt PROG OUT gt lt CODE gt lt MARKERS gt lt SSV gt User manual Endurance to program a pause max 9 hours 59 minutes 59 seconds During the pause the needle will move to home position if the previous step is an aspirate or dispense action If you want the needle to stay in the same position an aspirate or dispense step of 0 uL must be programmed at the desired position to activate the compressor to put air pressure on a sample The compressor will stay active until it is switched off in a next programmed step The compressor will be automatically switched off at the end of the
90. ons per vial maximum value is 9 injection volume can be entered for each injection per vial The maximum programmable injection volumes are 38 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance partial loopfill 50 of the programmed loop volume uL pick up injection volume loop volume 3 x needle volume 2 full loop not programmable is egual to the loop volume but needs more sample to fill the loop 3 x loop volume for loop volumes lt 100 uL 2 x loop volume for loop volumes 100 uL 499 uL 1 5 x loop volume for loop volumes gt 500 uL lt WASH gt Use this key to program wash methods It is possible to program a wash between injections samples or series For each wash method the volume of wash solvent can be defined The minimum programmable volume is 300 UL lt TIMEBASE gt if enabled in System Menu Usage Menu Press this key to enable control of the optional ISS valve and other devices via auxiliary or binary outputs A maximum of 5 timebase methods can be programmed The menu offers the following soft function keys lt AUX gt lt VALVES gt scroll through all program lines by pressing E or select AUX to move to the next auxiliary controls the ISS valve and the solvent selection valve The ISS valve can only be programmed if the optional ISS valve is installed 6 1 and 2 1 refer to the interconnected
91. pendix D Options and accessories 59 Appendix E Test procedures 61 Appendix F Injection valves 67 Appendix G Programming options 71 Appendix H Injection principles 73 Appendix 1 Trouble shooting 79 7 Ve oll GW mn Kol olole ce ree 83 Indek gcc cetaceans E a eee 93 vi 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Chapter 1 Introduction The Endurance is an autosampler that offers a wide variety of possibilities for HPLC It incorporates among other things the following features e suitable for use with various types of plates by various manufacturers e capable of executing full loop injections partial loopfill injections and uL pickup see section 1 1 below e accommodates use of various types of syringes volumes of 100 250 500 1000 UL or 10 mL e fully compatible with other laboratory equipment e designed for routine analysis and method development In addition options like plate cooling a second switching valve and a plate feeder see sect
92. r 3rd injection Escape to return to the Methods Menu 0060 183 21 27 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance To program the mix method Press keys Description lt MIX gt to enter the Mix Menu 1 E to define Mix method number 1 lt INSERT gt to define mix method step number 1 lt ASPIRATE gt 50 lt AIR gt E lt INSERT gt lt ASPIRATE gt 2250 Menu lt REAG A gt E lt INSERT gt lt DISPENSE gt 1800 gt gt 02 E lt INSERT gt lt DISPENSE gt 500 lt WASTE gt 5 E lt INSERT gt lt REPEAT gt 1 lt 4 4 E lt INSERT gt lt ASPIRATE gt 50 lt AIR gt E lt INSERT gt lt ASPIRATE gt 600 lt SAMPLE gt E lt INSERT gt lt DISPENSE gt 400 lt DESTINATION gt gt gt 2 E lt INSERT gt lt DISPENSE gt 500 lt WASTE gt gt 5 E lt INSERT gt lt ASPIRATE gt 500 lt AIR gt E lt INSERT gt lt ASPIRATE gt 2000 lt DESTINATION gt 3 E lt INSERT gt lt DISPENSE gt 2000 gt 9 E lt INSERT gt lt REPEAT gt 3 Escape Escape to aspirate an air segment of 5 0 uL to define mix method step number 2 to aspirate 225 0 uL to perform defined asp from reagent vial A to define mix method step number 3 to dispense 180 0 uL to destination well to define mix method step number 4 to dispense 50 0 uL to dispense defined volume to waste to define
93. rance Table of contents Chapter 1 Introduction siii vsi aii ket ooo ei volit aeo Naja 1 1 1 Injection principle e nan 1 1 2 Front view of the Endurance en 2 1 3 Back view of the Endurance enn 3 1 4 Keypad and display of the Endurance 4 Chapter 2 Preparations for use 7 2 1 HPLC connections eenannnn 7 2 2 Waste tub JI vas iji cers dari Areni rea ooo ei ei ee ke fen 8 2 3 Wash solVeNt viii ie irena sie dete ieee eee aetna 8 ZA SYNGE i v sie date oditi pivi leat joda vika ne A dient Dona se leon 9 2 5 Needle assembly nannaennna 10 2 6 Optional needles nana 11 2 7 Combination of syringe sample loop and buffer tubing 11 2 8 Plates and sample handling 0 cc eeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeenaees 14 2 9 Placing reagent vials transport vials 15 2 10 Plate lt 1 16 eee eee ee ee 15 Chapter 3 Getting started ooo ccccs ce cssesteseseeteseseeseseeeesesesneneeeesenes 19 3 1 Menus of the Endurance eeececeeeeteeeeeeeneeeeeetaeeeeeeaeeeeeenaeeeeneae 19 3 2 Convenient working order ccecceceeeeseeeeeeeeeeeeeeeeeaeeeenaeeeeeeeeaes 20 3 3 Types of Methods and links to Series 20 3 4 Executing a Series ccceecseeescec
94. rance will stop if an empty space is encountered during the run an error code will be generated e air segment decide whether an air segment will be used for analytical runs for explanation of air segment refer to Appendix H e headspace pressure to switch headspace pressure on or off The Endurance uses headspace pressure to facilitate transport of sample into the loop The compressor will always be used during a wash procedure Please note that accuracy and reproducibility may decrease if headspace pressure is switched off However headspace pressure will only be useful if sample wells are airtight refer to sections 2 5 and 2 8 time display offers a choice between two types of time representation key click error beep and alarm buzzer offer the possibility to switch sound signals on or off Table 5 1 Overview of General settings General setting for default possible range Loop volume 100 uL 5 1000 uL Needle tubing 15 uL 1 200 uL Syringe volume 250 uL 100 250 500 1000 uL or 10 mL Syringe speed normal low normal or high Scale factor 1 0 0 1 1 0 needle height 5mm 0 40 mm skip missing vials yes yes or no air segment yes yes or no headspace pressure no yes or no time base display HH MM SS H MM SS or H MM mm key click on on or off error beep on on or off alarm buzzer on on or off Artisan Technology Group Quality Instrumentation 0060 183 21 Guaranteed 888 88 SOURCE www arti
95. re in those cases System Menu General Menu 1 Fingertight nut and ferrule Needle tubing Needle connection nut Standard sample needle Needle holder Air outlet nut E cee V Prepuncturing needle E nee Co Sensor detects plate height missing plate and missing vials E Loosen the needle connection nut 3 2 Loosen the fingertight nut and ferrule 1 O 3 Carefully pull out sample needle and tubing 4 Insert anew sample needle and tube through the ee needle holder 5 and tighten the nut 4 did 5 Connect the other end of the tube to port 4 of the Figure 2 3 Needle assembly injection valve using a fingertight nut and ferrule Do not tighten too much to prevent block of tubing 6 Lower the cover of the Endurance 7 Check sample needle height default height 5 mm from plate If necessary adjust the value in the System Menu General Menu refer to Chapter 5 8 Select soft function key lt WASH gt in the Ready Menu to clean the new sample needle 10 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 2 6 Optional Needles Needles of the following types can be installed in the Endurance e LSV needle sample needle with large inner diameter for viscous samples or in case large volum
96. s The switching time of the injection valve exceeds 500 msec ISS A valve is not in a valid position The ISS A valve did not switch within 1 5 seconds ISS B valve is not in a valid position The ISS B valve did not switch within 1 5 seconds Syringe dispenser unit ERROR 21 ERROR 22 ERROR 23 ERROR 24 ERROR 25 The syringe valve did not switch The syringe did not reach home position in time The syringe spindle did not make the correct number of rotations The spindle does not rotate The syringe valve did not find a valid position Injection needle unit ERROR 30 The sample needle arm did not reach or leave home position vertical ERROR 31 The sample needle arm is in an invalid horizontal position while moving down ERROR 32 The sample needle arm did not reach or leave destination within a certain time horizontal ERROR 34 Sample needle arm not in vertical home position while moving horizontally ERROR 39 Vial sensor sticks ERROR 40 The sample needle spindle does not rotate correctly ERROR 41 The sample needle did not reach or leave home position ERROR 42 The sample needle is not at home position ERROR 53 The sample needle arm is not in the home position while moving the plate Plate ERROR 58 Not enough plates in right lift to execute run of series ERROR 59 Missing plate 0060 183 21 57 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User m
97. s is performed A 01 At the end of the defined analysis time the Ready Menu will be displayed again to indicate that the Endurance is ready for the next analytical run 24 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Example 2 A 3 x 10 uL injection with uL pick up wash between injections In this example a different injection method is used than in the previous one For that reason several settings must be adapted in the System Menu For system settings Press keys Description System to enter the System Menu lt GENERAL gt E to enter the General Menu E until Air segment appears to go to the Air segment field lt NO gt E to switch off air segment Escape to return to the System Menu lt PLATES gt E to enter the Plates Menu EE to go to transport vials field 1 E to define position of the first transport vial 1 to define position of the last transport vial Escape Escape to return to the Ready Menu To program a method Press keys Description Methods to enter the Methods Menu lt INJECTION gt 02 E to define method number 02 lt PICK UP gt E to select the injection mode for this method 100 E to define the analysis time 3 E to define the number of injections per well 100 E to define volume of 10 0 uL for 1st injection 100 E to define volume of 10 0 uL for 2nd injection
98. santg com User manual Endurance lt USAGE gt Press this key to enter the following Usage settings e protection code to enter a code for protection of methods Enter a six digit code 000000 999999 for protection of all methods Press CL to erase the code If a code has been defined it is not possible to enter the System Menu and the programming menus without entering the protection code Default none e timebase methods to enable or disable the possibility to program timebase methods The Endurance controls other connected equipment during analysis time Program timebase methods in the Methods Menu Default disabled e mix methods to enable or disable the possibility to program mix methods for the Endurance Program mix methods in the Methods Menu Please note that the Endurance cannot analyze priority samples during a run if the mix method is enabled Default disabled e user program to enable or disable the possibility to program a user program If this function is enabled it is possible to enter a user program protection code 6 digits Program the user program in the Methods Menu Please note that the Endurance cannot analyze priority samples during a run if the user program is enabled Default disabled e labeled wells to enable or disable the possibility to program labeled wells Program the location of labelled wells in the Series Menu Default disabled e templates to enable or disable the possibility to progra
99. ss Escape twice to return to the Ready Menu until the lift is full press Escape to return to the Ready Menu 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Keep in mind that the plate that is on the plate holder in the Endurance is number 1 the plates on the lift are numbered 2 through 7 The uppermost plate in the lift is number 2 The Feeder is now ready for use The left lift is used for storage of plates that have been processed and for plate switching seguences At the end of the programmed series Endurance will make sure that plate number 1 is always on bottom of the left lift and the plate with the highest number will be on the plate holder Example If 7 plates are used plate number 7 will be on the plate holder at the end of the programmed series plate number 1 will be at the bottom of the left lift plate number 2 will be on top of number 1 and the uppermost plate in the left lift will be number 6 Make sure that the tray holder of the Endurance always contains a plate at the start of programming a series CAUTION 8 Figure 2 4 Feeder option 1 Grab head 4 Drain wash position 2 Right lift 5 Condensed water and leakage 3 Plates in right lift 6 Left lift 0060 183 21 17 Artisan Technology Group Quality Instrumentation Guaranteed
100. syringe at this moment and tell the system not to display this message again the message will not be displayed again until 50 000 more syringe actions have been counted Syringe valve will have to be replaced and the counter for valve actions will have to be reset by the maintenance engineer lt DEFAULT ALL gt To change all software settings to default All series methods templates and the user program unless protected by protection code will be erased If lt DEFAULT ALL gt is selected check whether hardware configuration still is compatible with settings entered in the System Menu lt SSV gt option Use this key to start a procedure in which all lines of the solvent selection valve can be primed The menu offers the following possibilities lt SSV1 gt to To open the corresponding port of the solvent selection valve lt SSV6 gt lt PRIME gt To prime the selected solvent line with one syringe volume The last selected port will remain active after leaving the SSV mode lt COOL gt option Use this key to enter the programming mode for Peltier plate cooling The programmable temperature range is 4 C to 40 C The maximum cooling capacity is approximately 20 C below ambient refer to Appendix B for specifications Connect the condensed water and leakage connector see figure 1 1 number 11 to a waste container on the floor to drain condensed water If the cool option is switched lt ON gt the following soft fu
101. t 4 lt HOME gt 40 HPLC connections 7 0060 183 21 Artisan Technology Group Quality Instrumentation 93 Guaranteed 888 88 SOURCE www artisantg com User manual Endurance I initialization 51 lt INJECT gt 40 lt INJECTION gt 38 39 injection principle 1 71 76 injection method 20 number 37 injection volume 11 13 38 39 inject marker pulse length 36 INPUT 1 4 47 48 input edge next injection 36 input edge next well 36 lt INSERT gt 37 40 installation 7 51 52 Interrupt 4 introduction 1 5 lt lO gt 36 I O connections 3 45 48 ISS 39 K key click 34 keypad 4 5 keys 4 5 L labeled well 35 43 labeled well marker pulse length 36 last transport vial 35 lt LEFT LIFT gt 15 31 lift 15 17 31 lt LIFT DOWN gt 16 lt LIFT HOME gt 31 lt LIFT UP gt 16 lt LOAD gt 40 lt LOG gt 32 logbooks 81 89 loop volume 33 34 performance check 64 lt LOW gt 41 LSV needle 11 M mains input 3 mains switch 3 lt MANUAL gt 33 lt MARKERS gt 41 45 MENU 5 19 Menu 5 19 Methods 5 19 20 21 lt METHODS gt 37 42 lt INJECTION gt 38 39 lt MIX gt 37 38 lt TIMEBASE gt 39 lt USER PROGRAM gt 40 42 lt WASH gt 39 Methods Menu 19 37 42 missing plate detection 10 14 missing vials detection 10 14 lt MIX gt 37 38 mix method 20 37 enable disable 35 number 37 MN 5 19 N needle 2 10 height 34 37 38 40 holder 10 prepuncturing 10 14 repl
102. the edge sensitive inputs for the next injection e input edge next well to define the edge sensitive inputs for the next well e freeze input active to define whether the freeze input is active when high or freeze input is active when low e reset outputs after last series to determine whether the outputs should be reset to default after the last series Refer to Chapter 6 for more specific information on I O connections Table 5 2 Overview I O menu possibility default range inject marker pulse length 1 0s 0 1 2 0 well marker pulse length 1 0s 0 1 2 0 labeled well marker pulse length 1 0s 0 1 2 0 input edge next injection falling falling or rising input edge next well falling falling or rising freeze input active low low or high reset outputs after last series no yes or no lt CLOCK gt Use this key to switch the system clock on or off Select ON to enter the clock menu in which you can set date yy mm dd and time hh mm This date and time will be displayed in the Ready Menu lt COMM gt Use this key to define a device identifier for communication with other equipment e g a PC An identifier between 20 and 29 can be selected for the Endurance 36 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance 5 3 Methods Menu This menu allows the user to program various types of methods it is possible to define 24
103. the equipment A Removal of panels may expose users to dangerous voltages Disconnect the Endurance from all power sources before removing protective panels Always replace blown fuses with fuses of the size and rating indicated on the fuse panel and holder Refer to Appendix B of this manual for more information on fuses Replace or repair faulty insulation on power cords Check that the actual power voltage is the same as the voltage for which the Endurance is wired Make sure power cords are connected to correct voltage sources The Endurance must only be used with appliances and power sources with proper protective grounding 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Q e Perform periodic leak checks on supply lines e Do not allow flammable and or toxic solvents to accumulate Follow a regulated approved waste disposal program Never dispose of flammable and or toxic solvents through the municipal sewage system e Using the Endurance in other ways than indicated in the instructions given in this manual may cause unsafe conditions 0060 183 21 iii Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance iv 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endu
104. these examples to learn to work with the Endurance These examples can be executed after the Endurance has been installed in accordance with Appendix A and after all items described in Chapter 2 have been correctly set up Example 1 A 10 uL partial loopfill injection After the Endurance has been switched on an initialization procedure is executed In this example it is assumed that a loop of 100 uL needle tubing of 15 uL and a syringe of 250 uL has been installed Wait until the Ready Menu appears on the screen then execute the following steps For system settings Press keys Description System to enter the System Menu lt GENERAL gt E to enter the General Menu 0100 E to define the volume of the installed loop 015 E to define the volume of the needle tubing lt 250 gt E to define the volume of the syringe lt NORMAL gt E to set syringe speed to normal 05 E to set sample needle height to 5 mm lt YES gt E to enable use of air segment lt NO gt E to switch off headspace pressure Escape to return to the System Menu lt PLATES gt E to enter the Plates Menu lt 96 LOW gt to define the type of plate to be used lt IN ROWS gt to define the processing order of wells Escape Escape to return to the Ready Menu For this example all other settings used will be default 0060 183 21 23 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual En
105. tion method number Wash method number OTime base methods number O Mix method number Time base and mix method are only available if enabled in the System Menu O Use calibration vial number 4 Yes No O No of samples between calibration The calibration vial is only available if enabled in the System Menu not available if Mix Method has been programmed O Plate number if Feeder option is installed First sample well Last sample well Only if a mix method has been programmed or if used in user program O First destination well O Vial Reagent A O Vial Reagent B O Vial Reagent C O Vial Reagent D Only if the use of labeled wells has been enabled in the System Menu O Labeled well no 1 O Labeled well no 2 O Labeled well no 3 O Labeled well no 4 marked questions are always asked in series O marked questions depend on the used methods and the settings entered in the System Menu Explanation After you have entered the required settings in the System Menu and after you have programmed methods to be used for an analytical run you can press Series to enter the Series Menu Table 5 4 gives an overview of the items you have to define for the Series e With Templates If you are going to execute an analytical run by way of a template you will only be asked to enter the template number and to indicate the location of the first sample well and the last sample well 0060 183 21 43 Artisan Technology Group
106. tions it is very important that samples are properly handled Note the following e Standard wells can best be filled by means of a narrow end pipette to allow air to escape when filling the well e Do not fill wells to the rim as sample might be forced into the prepuncturing needle causing cross contamination of samples and contamination of the sample needle e Forvials make sure the seals are airtight to prevent air bubbles in the sample and prevent evaporation of volatile samples check seals after crimping if the cap can be turned easily the seal is not airtight and the handcrimper should be adjusted If wells are used that are not airtight switch off headspace pressure in the System Menu General Menu Check whether the needle height is sufficient for the new type of plate that is installed System Menu General Menu Adjust if necessary Execute the following steps to replace a plate in the Endurance 1 Select soft function key lt EXCHANGE gt in the Ready Menu if Feeder option is installed select lt PLATES gt and select lt EXCHANGE gt The plate moves to the left 2 Take out the plate and replace it by another one 3 Select soft function key lt PLATE HOME gt The plate moves to operating position again If you have replaced the plate by a plate of the same type you are now ready If you have installed a new type of plate execute the following steps 4 Press System 5 Select soft function key lt PLATES gt
107. to install the 250 mL wash solvent bottle 1 Fill the wash solvent bottle with the appropriate wash solvent Use of methanol organic solvent lei no buffers or a mixture of water and isopropanol 80 20 is recommended Before using the wash solvent degas it with Helium or an ultrasonic bath F 2 Screw the bottle to the cap in the holder 3 Place the holder in the Endurance as indicated in figure 2 1 4 Putthe wash solvent tube in the wash solvent 5 Lower the cover of the Endurance 2 6 Select soft function key lt SYR END gt in the Ready Menu to fill the syringe 7 Place the syringe back in home position by selecting soft function key lt SYR HOME gt Fiaure 2 1 Wash solvent bottle 8 Repeat steps 6 and 7 until the wash solvent tube and the syringe are completely filled 9 Select soft function key lt WASH gt to perform a standard wash routine 10 If any air remains in the syringe select lt SYR END gt again to fill the syringe with wash solvent press lt SYR HOME gt again to move contents to waste Repeat if there is still air in the syringe and gently tap the syringe as wash solvent is dispensed to waste 8 0060 183 21 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance If you use an application that reguires more than 250 mL of wash solvent for a complete run install a longer tube with fla
108. uid The programmed injection volume is aspirated from the sample well lt a Syringe Column gt Transport liquid Sample The sample needle moves back to the transport vial The sample is quantitatively transported into the loop with tum gt transport liquid mobile phase from the transport vial Tronsport liquid The injection valve is switched to INJECT The sample loop is now part of the HPLC mobile phase flow path sample is transported to the column The analysis time lt 5 Sinje gt Starts to run Transport liquid 1 Sample 0060 183 21 77 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance The next seguence will skip the first withdrawal of transport solvent unless a wash routine is performed or the Endurance has emptied the buffer tubing to waste In those cases the sequence is completely repeated Air segment If an air segment has been programmed it appears at the front of the first plug of transport liquid and at the front of every sample plug Use of an air segment can be enabled in the System Menu General Menu Note The air segment at the front of the sample plug is injected into the HPLC system Needle Injection loop Buffer tubing A Transport Sample Air i Eluert Transport Air gt RN S gt
109. use a different order however you should keep in mind that settings entered in the System Menu determine which possibilities appear in the Methods and Series menus Refer to chapter 5 for more information on specific items in menus and the way they influence the other menus 3 3 Types of Methods and links to Series The Endurance offers the following types of methods for different parts of the sample handling routine e injection method contains information on the injection routine flush volume and analysis time e wash method describes a wash volume and when a wash must be executed e mix method a pre injection method in which additional sample handling can be performed e g pre column derivatization e timebase method a post injection method with which outputs to other devices e g integrator or pump and switching of the ISS valve are controlled e user program offers the possibility to program seguences of all actions that can be executed by the Endurance in separate steps Each programmed method is assigned a number The Endurance offers the possibility to store a combination of defined methods in a template A template is also identified by a number Methods must be linked to series before they can be used The following possibilities are offered by the Endurance e You can assign an individual method to a series methods mix injection wash timebase can be linked to wells in a series e You can assign a templat
110. ven Plate feeder User manual Endurance Next injection input Next well input Freeze input Stop I O 4 Programmable inputs RS232C or RS422 or RS485 Microsoft Windows 95 Windows NT Yes Built in Peltier cooling processing unit Programmable Range 4 C 40 C Cooling capacity Ambient 20 C measured on cooling plate One optional high pressure 6 port valve 6 way integrated solvent selection valve Rheodyne 9000 series biocompatible valve with PEEK sample needle and PEEK loop One optional Rheodyne or Valco biocompatible high pressure 6 port valve Mistral column oven combined with the Endurance The injection valve and optional high pressure valve fit into the column oven For feeding an additional 6 low plates 96 low 384 low or 2 high 96 high to the Endurance The Feeder is attached to the front of the Endurance This means an extra 175 mm depth added to the Endurance width 280 mm total depth 575 mm 0060 183 21 55 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Figure B 1 127 5 40 25 OOODOOOOB OO ZOFEQ O O O O O O O OOOODDOOOD OOQ O O Q O O O Q O OO OPOOODEB A xD ty
111. x SSV 8x CODE OUT END TIME destination vaste reagent REPEAT WAIT WASH Series Use cal Nr 4 yes no calibration interval Plate number Note Sample wells These parameters depend on the content of the ination Rod methods used and or the System Settings of the eagent wells Labeled wells Endurance Start Stop e First series Note e Last series Optional Soft function keys lt START gt lt REMOTE gt Priority e Note only if Feeder option is installed Well number PRIORITY Interrupt Not used Only available when user program and mix method have been disabled in the System Help Context and status sensitive help screen if available Settings 0060 183 21 71 Artisan Technology Group Quality Instrumentation Guaranteed 888 88 SOURCE www artisantg com User manual Endurance Ready Menu lt Menu gt lt WASH gt lt SYR END gt lt UTILS gt lt SERIAL gt lt SSV gt lt COOL gt lt SERVICE gt lt EXCHANGE gt lt PLATES gt Cool ON OFF lt COPY lt ERASE gt lt LOG gt lt DEFAULTALL gt Setpoint Switch ON OFF Exchange Perform Move syringe Copy method Erase methods Logbook All methods Communication Prime solvent Service mode Lift left standard wash 8 Userprog erased all settings protocol valve Lift righ to default Plate k System Settings System Menu gt lt GENERAL gt lt USAGE gt lt PLATES gt

Chapter 4. Using the Endurance

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