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S 5200 Autosampler User Manual

1. FUNCTION KEYS Ti 1 S US return to Status Screen U F5 PRIO SAMPLE Show Priority Sample Menu Version 3 2 April 2007 37 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 7 5 ANALYSIS PROGRAM MENU The analysis program is selected by using the Main Menu and key 3 In this menu all for the analysis important parameters are entered It is possible to store a multitude of different programs which can be individually selected by entering the number of the program acr SANPLE gt ANALYSTS PROGRAIM no 1 INJECTION VOLUME INJECTIONS VIAL WASH PROGRAM SYRINGE SPEED NEEDLE DEPTH ANALYSIS TIME SAMPLE TEMPERATURE AIR SEGMENT Picture 20 Analysis Program Menu DESCRIPTION The Analysis Program Menu displays the following information InNO The number of the analysis program tobe edited in INJECTION VOLUME This value is dependent on the currently selected volume mode The mode can be changed with the F2 function key and is displayed on the right upper corner of the content area Variable Volume Enter the injection volume in ul Fix Volume Enter the number of times the sample loop should overfilled e g 3 times Note that the variable volume mode is only available with the variable volume injection option INJECTIONS VIAL Enter the number of injecti
2. Picture 29 Derivatisation Example Reagent A 5 ml Vial Reagent B 5 ml Vial Reagent C 5 ml Vial Sample Vials 61 63 Empty Vials 1 3 ar wn After the placement of the vials the user has to setup the instrument s programs as outlined below Version 3 2 April 2007 Page 53 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler ANALYSIS PROGRAM In the ANALYSIS PROGRAM menu the user selects program number 4 for storing it Then he enters all parameters according to his samples method Volume Mode Variable Injection Volume 10 ul Injections Vial 3 Time 20 minutes HA WN Wash Program 1 SAMPLE SEQUENCE In the SAMPLE SEQUENCE menu the user specifies the sequence according to the diagram above From 61 63 Prog 4 DERIVATISATION PROGRAM The last step the user has to conduct is editing the Derivatisation Program In the DERIVATISATION PROGRAM menu he enters the following 1 Sample 30 ul Reag A 10 ul Mixing 4 x React Time 10 sec Reag B 20 ul Mixing 5 x React Time 10 sec Reag C 10 ul Mixing 4 x React Time 5 sec Dilution 70 ul 50 dilution 70 ul total volume of Sample Reagents Wash after each Injection YES A Uh Q Q Uh Q Air Segment 3 Version 3 2 April 2007 Page 54 74 OPERATION MANUAL
3. 30 MenlEOCK 5 oS le SSeS eI Ce e C e LR BGB LI BS BEES 32 Menu eite ie eR e e e E Ee e E E P eh ied 33 Status awe ears ear aa i a i MI EI AME MILLE ee 34 MENU 36 Sample Sequence 37 Analysis Program s sn 38 Mial EISEMOHUS Se ie ie eb aad 40 Auxillary Functions Menu ass a a a a a a n an an un aQ aQ aha a be ha oa 41 iid fii is N ii 43 Instrument Configuration Menu e a a e o a dba ud 45 snam 47 Service as 49 DEVICE ttuitttuiettte 51 Derivatisation Vial Positions 52 53 Sampl Rack POSION Sisena anana D n D 62 63 5 64 Injection Valve Diagtram 5 hif d af abe f a af aa af a afa IC 67 Version 3 2 April 2007 Page 4 74 OPERA
4. NEEDLE POSITION The injection position of the sample needle in the inject port must be exactly in the middle A not correctly adjusted sample needle can cause premature abrasion of the needle and seal In case of a defect needle port seal or block up of a capillary the sample volume is not injected completely leaking of the injection port A drop remains on the injection position The injection needle should also be checked concerning any damage BLOCK UP OF A CAPILLARY The transfer of the sample into the needle transfer capillary can be checked with the help of colored solution and programmable air segments With a syringe each capillary can be checked at the injection valve and any blockage can be removed Version 3 2 April 2007 Page 71 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler BLOCK UP OF INJECTION NEEDLE The transfer can be checked as described above When no liquid shows up in the transfer capillary the needle may be blocked This blockages can be easily removed by pushing a small gauge wire through the Injection needle from top to bottom to push out any particles inside the needle 11 2 VIAL ERROR In case the error message EVIAL will be displayed although a vial is placed in this vial position the needle has to be checked If necessary the needle has to be exchanged as a defective needle can pull out the vial from the rack and the sample arm can be jammed
5. or directly enter the menu with key 5 S Move the cursor down to the OPERATION MODE field Using the SEL UP and SEL DOWN keys will change between the different modes Select the EXTERN mode Now the instrument is controlled via digital signals of an external controller 9 2 4 SERIAL OPERATION When selecting the serial mode the autosampler is controlled with the help of an external software e g ChromStar S press the MENU key S move the cursor to the INSTRUMENT CONFIGURATION MENU and press ENTER or directly enter the menu with key 5 S move the cursor down to the OPERATION MODE field Using the SEL UP and SEL DOWN keys will change between the different modes Select the SERIAL mode Now the instrument is controlled by RS 232 serial commands S press the F1 key to enter the STATUS SCREEN This is very important as the 5200 has to be in the STATUS SCREEN when serial communication from a PC is started S now the data system can control the autosampler 9 2 5 AUXILIARY FUNCTIONS The S5200 features an auxiliary port with 5 separate analog outputs These can be used to control external instruments like motor valves The individual output No 1 to 5 can be programmed in the AUXILIARY FUNCTIONS Menu 7 7 NOTE Auxiliary Function No 1 is pre defined when the Wait Time is activated see SPECIAL FUNCTION below Version 3 2 April 2007 Page 57 74 OPERATION MANUAL Schambeck SFD GmbH
6. Instrument Description 17 oT Generale remet 17 6 2 Systemi Des oripti ft tette i EE 18 6 2 1 MeGhanl6S 18 06 22 Sampling 19 6 3 Working Principle Variable 23 6 3 1 Taking the Sample aussi eked QQ nee 23 6 3 2 Transfer to the Sample Loop 25 6 3 3 Sample u ae tet Q Q ea Q ma Q Qu Q aQ Q ga Q teret us 26 06 3 4 Washing yasa sm sa n aQ eee EID Ee Dette teet tus 26 Y Screen MENUS pm C 28 7 1 Man BRIAN EEUU UR EU ERES 30 Z kaj Main Men Lock ERE EE EE UE EE EE E EE 32 Ave Men Unlock d EE T 33 1 2 SlALUS a 34 T 9 Priority Sample Menu 1 2 2 81 sd dd i Hd Md HH 36 7T 4 Sample Sequence Meriu 2238 DINH UN AH a d i
7. P ALe eNA EAER ONAE NPR SNDE EAR ENT ENR SRE E EEEE EE EE SEEE E E EE E E EE EE E EEE EEE a SEEE AE E E E EE EA SEAE EN ESA E AE EE EAEE AEE TE mU E ee in TIME DATE At the upper right corner of the content area the individual time and date positions be changed by using the CURSOR keys After entering the new time date the ENTER key has to be pressed WAIT TIME INJECTION Here you can enter a wait time before each injection If a wait time is entered the Aux Functions 1 and 2 are occupied and cannot be used for custom purposes SYRINGE VOLUME This is the volume ul of the syringe used Only change this value if you install new syringe SAMPLE LOOP This is the volume ul of the installed sample loop You can change this value if you install an other sample loop ELUENT SEGMENT The Eluent Segment is a specific volume of wash solution for delivering the sample into the sample loop 5 15 ul Ff Version 3 2 April 2007 Page 45 74 Schambeck SFD GmbH Rh ndorfer Strasse 51 53604 Bad Honnef OPERATION MANUAL S 5200 Autosampler n SAMPLE COOLING n TIME SCALE n OPERATION MODE n PULSE DURATION FUNCTION KEYS F2 SERVICE PROG 1 u F3 DIALOGUE GERMAN F4 SERVICE PROG 3 F5 PRIO SAMPLE Version 3 2 April 2007 Description eee STATUS Variable Volume 35 40 ul
8. Rh ndorfer Strasse 51 53604 Bad Honnef S 5200 Autosampler SPECIAL FUNCTION When a Wait Time gt 0 is programmed Auxiliary Function No 1 AF1 is used in a certain way The AF1 signal is activated as soon as the START key is pressed this signal can be used to start an external instrument like a gradient pump When a Wait Time of 0 is programmed AF1 is dormant and can be programmed otherwise in the AUXILIARY FUNCTIONS Menu 7 7 Version 3 2 April 2007 Page 58 74 OPERATION MANUAL S 5200 Autosampler Schambeck SFD GmbH Rh ndorfer Strasse 51 53604 Bad Honnef 9 3 ERROR MESSAGES In case of an error a short error code is shown in the top right corner of the status area Display EVIAL EVSEQ EDVNO EDRCK EVPRG EMOTX EMOTY EMOTZ EMOTS Error Syringe Volume Error Undefined Error Vial Error Vial Sequence Error Derivatisation Vial in wrong rack Derivatisation Rack Error HARDWARE ERRORS Injection Valve Error 3 Way Valve Error X Axis Motor Error Y Axis Motor Error Z Axis Motor Error Syringe Motor Error Description LOGICAL OPERATIONAL ERRORS Syringe volume was exceeded or other unknown error Vial sensor detected a missing vial at the specified position A logical error of the Sample Sequence occurred The Vial programmed in
9. Schambeck SFD GmbH Rh ndorfer Strasse 51 2 S 5200 Autosampler 9 OPERATION 9 1 PROGRAMS Hereby stepwise procedures for various often needed operations are described Please note these are only suggestions no defined instruction procedures 9 1 1 ANALYSIS PROGRAM First you have to enter an Analysis Program to be used for the sample sequence s s press MENU key move the cursor to the Analysis Program and press ENTER or directly enter the menu with the 3 key move the cursor to the NO field and enter the program number under which this Analysis Program will be stored e g 3 move the cursor to the INJECTION VOLUME field Enter the injection volume variable injection volume or the multiplier by which the sample loop should be over filled fix volume injection with multiple injection enter the injections to be done per vial move the cursor to wash program and enter the no of the wash program to be used e g 3 move the cursor to the SYRINGE SPEED field and select 50 move to the NEEDLE DEPTH field and check if the needle depth is appropriate for the used vials 2ml conical plastic vials 39mm 1 5ml glass vials 30mm move the cursor to the ANALYSIS TIME field and enter the time duration for a single analysis with upgrade option cooling heating enter the temperature in case the heating cooling option should be switched off enter 0 move the cursor to
10. available dosage through stepper motor driven 500 ul glass syringe stainless steel optional PEEK lt 0 5 with 100 ul fixed volume injection method lt 1 0 with 20 ul variable volume injection mode lt 0 01 dependent on selected washing program programmable wash cycles and volume up to 9999 programmable time base selectable in 1 min 0 1 min or in seconds standard 2 racks for 60 vials 1 5 ml each other racks on request 230 V 110 V 50 60 Hz 230 V 2x 1 0 AT 110 V 2x 2 0 AT 10 35 G 415 x300 x445 mm Hx W x D 20 kg 9 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 2 S 5200 Autosampler 4 INSTALLATION 4 1 components single elements which be individually used combined to complex module system This ensures an optimum system arrangement of the individual instruments depending on the application requested For the Autosampler S 5200 a space of 350 x 450 mm is required It is recommended that the rear side as well as the right side of the instrument remains accessible for exchanging the wash solvent and or sample loop 4 2 TRANSPORTATION SAFETY For transportation purposes a safety catch has been mounted on the moving sample arm Before starting the instrument remove this safety catch Open the Autosampler s cover remove the red safety catch by removing the 4 screws remove the red safety band by cu
11. injection option F3 AUX FUNCT Switch to the Auxiliary Functions Menu F4 VIAL LIST Switch to the Vial List Menu Version 3 2 April 2007 Page 39 74 Schambeck SFD GmbH OPERATION MANUAL Rh ndorfer Strasse 51 53604 Bad Honnef S 5200 Autosampler 7 6 VIAL LIST MENU This submenu can be selected by pressing the F4 With variable volume injection operation itis possible to program different sample volumes taken from the same sample vial With this function automatic calibration functions can be programmed without additional dilution acr VIAL LIST PER INJECTION USE LIST NO INJECTION Picture 21 Vial List Menu DESCRIPTION The Vial List Menu displays the following information in PROG The number of the vial list to be edited and or used USE LIST Here you can select if this list should be used in the analysis or not I INJECTION This column specifies the respective injection number Enter the desired injection volume in this column FUNCTION KEYS key SS STATUS reumtoStusSoeen 000000000 F4 ANALYSIS PROGRAM Return to the Analysis Program Menu x F5 PRIO SAMPLE Show Priority Sample Menu Version 3 2 April 2007 Page 40 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 7 7 AUXILIARY FUNCTIONS MENU The auxiliary function program is selected from the
12. the sample loop has to be exchanged s Remove the side cover on the right side of the instrument where the syringe and injection valve is positioned 5 Remove the connections of port 1 and 4 of the injection valve Unscrew the sample loop The new sample loop with the appropriate fittings and ferrules has to be mounted to port 1 and 4 Important For sample volumes higher than 100 ul the standard 500 ul syringe should also be exchanged for bigger one Version 3 2 April 2007 Page 66 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 2 S 5200 Autosampler 10 5 INJECTION VALVE MAINTENANCE Abrasion or any lines caused by particles in the fluid can cause leakages at the rotor or stator parts 10 5 1 DISASSEMBLING THE VALVE Disconnect the Autosampler from the power supply Loosen all fluid capillaries Cleanness is of the utmost importance when disassembling the valve Body gum Shaft Assembly Mt g r g gt gt sv Isolation Seal Rotor Seal Body Locating Pin i Stator Ring Stator Locating Pin a Stator Face PORT Assembly atte Stator Stator Support Ring PEEK version only Stator Screws 3 Picture 33 Injection Valve Diagram Unscrew the stator screws Remove the stator assembly by pulling axially to disengage the various parts Remove the rotor seal by prying it off o
13. 7 9 3 SERVICE PROGRAM 3 The service program is displayed by selecting the Service Program 1 and pressing the Function Key F4 Note The program can be only entered if the legitimation code PASS NO was set in the Service Program 1 In this submenu the Additional Volume for the sample injection can be set Normally stay with the default value of 20 ul ac SERVICE 3 PASS NO 123 ADDITIONAL VOLUME Picture 27 Service Menu 3 DESCRIPTION The Service Menu 2 displays the following information in ADDITIONAL VOLUME Display of the currently set Additional Volume This is the volume which is taken from a sample in addition to the programmed sample volume It is used to exactly move the sample to the beginning of the sample loop Y Y n Lu FUNCTION KEYS Description return to Status Screen 4 INSTR CONFIG Return to INSTRUMENT CONFIGURATION Menu F5 PRIO SAMPLE Show PRIORITY SAMPLE Menu Version 3 2 April 2007 51 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 53604 Bad Honnef S 5200 Autosampler 8 DERIVATISATION The derivatisation program is selected by using the MAIN MENU and key 6 or by using the cursor if the derivatisation option is available Otherwise the DERIVATISATION MENU is missing altogether The Autosampler is equipped with an automatic pre column derivatisation automatic samp
14. 77 50 055 Rotor Seal Injection Valve PEEK 31 01 011 Stepping Motor Syringe 23 02 001 Gear Belt Z Axis 23 02 002 Gear Belt X Axis 23 02 003 Gear Belt Y Axis 22 20 006 Sample Rack 1 2ml Vials Pos 01 60 22 20 007 Sample Rack 2 2ml Vials Pos 61 120 20 60 005 Front Glass Panel 12 2 SAMPLE LOOPS 12 2 1 PEEK Catalog Part 21 90 040 Sample Loop 5 ul PEEK 21 90 041 Sample Loop 10 PEEK 21 90 042 Sample Loop 20 ul PEEK 21 90 043 Sample Loop 50 ul PEEK 21 90 044 Sample Loop 100 ul PEEK 21 90 045 Sample Loop 200 ul PEEK Other sizes are available on request 12 2 2 STAINLESS STEEL Catalog Part Version 3 2 April 2007 Page 73 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 53604 Bad Honnef S 5200 Autosampler 77 55 020 77 55 021 77 55 022 77 55 023 77 55 024 77 55 025 Sample Loop 5 ul Stainless Steel Sample Loop 10 ul Stainless Steel Sample Loop 20 ul Stainless Steel Sample Loop 50 ul Stainless Steel Sample Loop 100 ul Stainless Steel Sample Loop 200 ul Stainless Steel Other sizes are available on request 12 3 SAMPLE VIALS Catalog Part 70 04 001 Sample Vial glass 1 ml w Crimp Cap Pack 100 pieces 70 04 002 Sample Vial conical 200 pl w Silicon Caps Pack 100 pieces 70 04 006 Sample Vials glass 1 5 ml Pack 100 pieces 70 04 101 Crimp Caps w Septum Pack 100 pieces 70 04 102 Silicon C
15. COnlttol s iii etta oti ont n i c tuc 57 9 2 4 Seral operaltlon n iioii eniti iet e niue 57 9 2 5 Auxiliary F i c i et c i c ad i te c ar i n 57 9 9 Error 2 1 pd D DL D DLE 59 10 Service 6 60 102 60 LOM 60 10 2 Replacing the Injection 62 10 3 Replacing the Injection 8 64 10 4 Replacing the sample Loop 4 2 2 2 2 2 S BERIBRRSHBERRRESHBERRRESHRERRRERHRE ER ERE E 66 10 5 Injection Valve Maintenance uu IRE REEL EE ELLE LEER e LEER ELE ee PEEL EE da 67 10 5 1 67 10 5 2 Heassembling the 68 10 6 Functio
16. End of Rack 1 Beginning of Rack 2 End of Rack 2 of WD 10 2 REPLACING THE INJECTION SYRINGE The standard version of the Autosampler is using a 500 ul syringe for sample dosing The piston of the syringe is linearly motor driven which ensures the accurate dosing process If very small large volumes should be analyzed the microliter syringe and the transfer capillary can be replaced Version 3 2 April 2007 Page 62 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH The top of the syringe is screwed into a 3 2 way switching valve With this valve the syringe can be connected either to the sample needle or to the wash solution The piston of the syringe is fixed to a forked support which is driven up and down To remove the syringe unscrew the knurled fitting 11 which fixes the plate spring holding the piston of the syringe Turn very carefully the glass syringe with a suitable spanner until it can be removed Fill the new syringe with dest water place the end of the piston under the forked support and screw the top end of the syringe into the 3 2 way switching valve Fix the end of the piston with the knurled fitting again To remove any air in the syringe an analysis run should be done followed by 6 to 7 washing cycles For checking the reproducibility of the measured values a multiple analysis run should be performed 3 Way Switching Valve Sample Wash Solution Po
17. Page 41 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 S 5200 Autosampler 53604 Bad Honnef automatically switched off STATIC When PULSE NO the output signal must be manually switched on and off FUNCTION KEYS F1 STATUS Return to the Status Screen F3 ANALYSIS PROGRAM Return to the Analysis Program Menu x F5 PRIO SAMPLE Show Priority Sample Menu Version 3 2 April 2007 Page 42 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 7 8 WASH PROGRAM MENU The wash program is selected by using the Main Menu and 4 It controls the wash functions before and or after the injection Several wash steps can be combined The wash program is activated through the analysis program SANPLE 2 WASH PROGRAM SYRINGE SPEED 100 SYRINGE VOLUME WASH STEP 1 TIMES WASH BEFORE EACH INJECTION NO WASH AFTER EACH INJECTION YES WASH AFTER EACH VIAL NO WASH POSITION INJ POS SAMPLE Picture 23 Wash Program Menu DESCRIPTION The Wash Program Menu displays the following information nN The number of the wash program to be edited SYRINGE SPEED Here you can change the speed of the syringe drive Possible values 100 50 and 33 SYRINGE VOLUME Specify the number of times the complete syringe WASH STEP volume should be used for each wash step WASH BEFORE EACH INJECTION Sel
18. be started as long as there are any errors displayed in this line iii i oe ee eee re ee ee eee eee ee ceed FUNCTION KEYS F2 VIAL E QUIT Clear any Vial Errors This has to be done before you can start a Sequence an any Vial are displayed F3 SEQUENCE RESET Reset the Sequence to start at the first vial first injection again Version 3 2 April 2007 Page 35 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 7 3 PRIORITY SANPLE MENU The priority sample screen is selected by Main Menu and 1 or directly by selecting the Function Key 5 Priority sample When activating the priority sample 5 the sample placed in vial position 120 will be injected immediately after the actual analysis is finished without stopping the current run For processing the priority sample a different analysis program no can be used If requested the vial position of the priority sample can be changed in the submenu This function is not possible during serial operation act PRIORITY SAIPLE ANALYSIS PROGRAM z PRIORITY SAMPLE INACTIVE FRIO S PRI0 S Picture 18 Priority Sample Menu DESCRIPTION The Priority Sample Menu displays the following information Le a a il EP rcM ici n ANALYSIS PROGRAM Enter the number of the Analysis Program to be u
19. c 4 6 DESCRIPTION You can select any of the displayed menus by moving the screen cursor to the appropriate menu using the CURSOR keys and pressing the ENTER key Alternately you can use the numeric keys 0 to 6 to access the menus directly The following menus can be access from the MAIN MENU aD a aaa a a a a a n STATUS Display the Status Screen also key F1 PRIORITY SAMPLE Display the Priority Sample Menu also key F5 SAMPLE SEQUENCE Show the Sample Sequence Menu ANALYSIS PROGRAM Show the Analysis Program Menu WASH PROGRAM Show the Wash Program Menu INSTRUMENT CONFIGURATION Show the Instrument Configuration Menu n DERIVATISATION MENU Show the Derivatisation Menu optional j Version 3 2 April 2007 Page 30 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler FUNCTION KEYS F1 STATUS Show the Status Screen F3 MENU LOCK Show the Main Lock Unlock Menu F5 PRIO SAMPLE Show the Priority Sample Menu Version 3 2 April 2007 Page 31 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 7 1 1 MAIN MENU LOCK All menus and settings can be protected against manipulations by illegitimated operators WAIN LOCK LEGITIMATION CODE Picture
20. can be removed from the top S The new sample needle has to be placed into the needle holder Use the pliers to tighten the needle insert and connect the capillary to the protruding end of the needle S Theinjection needle position has to be checked and adjusted For this please refer to the 70 1 Adjustment of Needle Position Version 3 2 April 2007 Page 64 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 52 S 5200 Autosampler Warning For this procedure the autosampler has to be connected to the power supply Please adhere strictly to the Service Menu description otherwise injuries can result if not correctly done s Afterwards the covering of the sliding carriage and the autosampler s cover have to be remounted clean the needle start the analyses which should be followed up by 6 7 wash cycles For checking the reproducibility of the system a succession of analysis runs should be performed Version 3 2 April 2007 Page 65 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 2 S 5200 Autosampler 10 4 REPLACING THE SAMPLE LOOP With variable injection volume the sample loop is only partially filled with sample If the fix volume injection mode is selected the sample volume to be injected is dependent on the size of the sample loop For extremely accurate dosage RSD lt 0 5 the sample loop should be overfilled with sample For smaller volumes
21. connection possibilities the autosampler can be integrated in totally different analysis systems At the back the bottle for the wash solvent necessary for flushing the system as well as the drain for not needed sample solution or used wash solution is positioned 9 REMOTE CONTROL WASHING SOLUTION COLUMN Picture 3 Back Side View 1 Wash Bottle Rack 7 RS 232 Serial Connector 2 Capillary Connections 8 Cooling Fan only w Cooling option 3 Connection DRAIN only w Cooling option 9 Power Switch 4 Connection DRAIN 10 Power Cable Connector 5 Aux Functions connector 11 Fuse Carrier w Voltage Selector 6 Remote Control Connector Version 3 2 April 2007 Page 14 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler 5 3 CAPILLARY CONNECTIONS WASH SOLUTION The 500 ml bottle for the wash solvent is placed into the special rack at the rear side of the instrument and has to be filled with the degassed wash solution The Teflon capillary has to be mounted with the fitting to the WASH SOLUTION connection The capillary must be put through the bottle s cap hole into the solution Note To ensure a correctly done wash cycle the bottle has to be filled with the wash solution and the end of the capillary has to reach into the wash solvent For most applications the eluent can be used as wash solvent Important The wash solvent eluent ha
22. measures exactly the sample volume selected The sample loop installed will be filled only partially with the selected sample volume and after turning the valve is transported to the separation column This injection technique allows the accurate dosage of the sample volume A programmed sample volume is sucked via the sample needle into the system Between the sample needle and the syringe a transfer capillary is installed which holds the measured sample volume until injection This avoids that any sample comes into the syringe which could cause any contamination For transportation of the measured sample volume into the injection system the sample needle is lowered into the inject port and is pushing the sample volume into the sample loop To secure the complete transfer of the sample segment a programmable eluent segment can be sucked on by the syringe With this eluent segment placed in front of the sample segment the sample can be transferred into the sample loop without any loss After the injection the eluent segment fills completely the capillary between the injection port and sample loop To avoid any mixing of the sample with the eluent segment an air segment can be programmed which keeps the two segments apart For standard application a sample loop of 20 ul is connected to the switching valve The Autosampler with variable injection mode can be used for both fix volume and variable volume injection operation When using the fi
23. z Sample Racks Washing Solution Picture 5 Working Principle Eluent Segment Then the 3 2 way valve positioned above the syringe switches to connect the syringe to the sample needle Now the desired air volume used for keeping the eluent and sample from each other apart is sucked on 3 2 Way Valve Air Segment Sample Racks Washing Solution Picture 6 Working Principle Air Segment Version 3 2 April 2007 Page 23 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 53604 Bad Honnef S 5200 Autosampler Now the needle is lowered down to the level programmed and the required sample volume Additional Volume programmed in Service Menu 3 is sucked on After the needle moves up again a second Air Segment is taken 3 2 Way Valve Sample Racks Washing Solution Picture 7 Working Principle Sample Note The max volume of the transfer capillary is 250 In case of higher volumes the autosampler has to be modified The length of the transfer capillary is exactly calculated so that the sample remains only in the capillary and is not sucked into the syringe Contamination or time consuming wash procedures of the syringe are eliminated Version 3 2 April 2007 Page 24 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler 6 3 2 TRANSFER THE SAMPLE LOOP The sample needle is positioned above the inject port and lo
24. 1 AUX 2 N C 12 AUX 3 N C 13 AUX 4 COM 14 AUX 4 N C 15 AUX 5 N C 8 7 6 5 4 3 2 1 e ON N e 15 14 13 12 11 10 9 Version 3 2 April 2007 70 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler 11 TROUBLESHOOTING 11 4 BAD REPRODUCIBILITY A bad reproducibility can have different causes like leakage block ups in the capillaries air bubbles in the injection port defective sealing ring in the inject port or not sufficiently degassed wash solvent The following points should be checked WASTE BOTTLE The waste bottle has to be positioned on the same height as the autosampler DEGASSING OF THE WASH SOLVENT Even very small air bubbles especially with small volumes can affect the reproducibility Therefore the wash solvent has to be degassed sufficiently before operation PROGRAMMING THE AIR SEGMENT The air segment is used for keeping the sample and the eluent segment apart from each other The volume of the air segment should be exactly selected to ensure the complete separation of the sample and the eluent segment but should not be injected With an air segment of 5 ul a reliable separation of the sample and eluent is secured CAPILLARIES Check all the fittings injection valve capillaries to the injection port connection to the sample needle connection to the separation column for any leakage
25. 15 Menu Lock DESCRIPTION To lock all menus enter the MENU LOCK menu by pressing F3 in the MAIN MENU and entering the legitimation code using the numeric keys When the code is confirmed with the key all menus and settings are locked until the system is unlocked again The Legitimation code is 23456 FUNCTION KEYS MAIN MENU Return to the Main Menu Version 3 2 April 2007 Page 32 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 7 1 2 MAIN MENU UNLOCK When the system is locked you first have to unlock all menus before you can make any changes to the system s parameters acr MAIN WENU UNLOCK LEGITIMATION CODE mm I 0 MENU Picture 16 Menu Unlock DESCRIPTION To unlock all menus enter the MENU UNLOCK menu by pressing F3 in the MAIN MENU and entering the legitimation code using the numeric keys When the code is confirmed with the ENTER key all menus and settings are unlocked again The Legitimation code is 23456 FUNCTION KEYS Page 33 74 Version 3 2 April 2007 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 7 2 STATUS SCREEN After pressing the F1 or 0 key in the MAIN MENU the Status of the system is shown on the screen All parameters important for the analysis are shown We recommend that this menu is displayed during
26. 5 5200 Autosampler User Manual Version 3 2 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 2 S 5200 Autosampler TABLE OF CONTENTS 1 Standard 1 u 5 1 1 Versions amp Upgrade ODptlos 5 rate 5 2 Safety Lini e M M 7 2 1 GeneraliElectrical Hazards t d E bee e E Peri cec eer eei terr i reu eoi et 7 2 2 General Precautions T Q Na orn 7 3 Technical Specifications u ianua naar rta dE ggg rand dona Eon a nua 9 e e e PORTET ToS 10 9 HA 10 4 2 Trarisportatiori Sat TJ 10 mun umaq m Q uu ua 10 A 3 Installation 2 ua p Pe 10 5 General Description 12 5 41 Front olde VISW unu mu u eerte dede dede den den d den de e He e RH EH E 12 5 1 34 Operation Panel imei tnt t a at t t HE HR d E HH T ETE HH TT TEE os 13 5 2 Back Side 14 5 9 Gapillary Contectiorts a neto menti re net re ne e na dne n 15 5 4 Gable ERROR RERO E REC RENE C T I 15 6
27. A bended needle also can cause any damage to the injection port 11 3 NO SAMPLE INJECTION CAN BE DETECTED Although sample injection is done no signal can be detected during data acquisition The function of the injection valve has to be checked in the appropriate service menu and the capillaries checked for any blockage If necessary the needle depth has to be checked for standard sample vials approx 30 mm The needle is not allowed to touch the bottom of the sample vial 11 4 BENT NEEDLE The injection needle does not bend under normal operation When this happens periodically the reason is most often that the needle does not reach its intended position and come down on some solid object like the sample trays The reason for this is dirt dust on the axis rails the movement of an axis is noisy and ends at different positions Clean the rails carefully and put some oil on them If this doe not solve the problem contact the manufacturer Version 3 2 April 2007 Page 72 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler 12 SPARE PARTS 8 ACCESSORIES 12 1 SPARE PARTS Catalog Part 20 21 920 Dosing Syringe 500 ul 20 34 003 3 Way Valve 20 20 044 Injection Needle 25 01 137 Air Needle 24 10 027 Injection Port Sealing 77 40 006 Injection Valve Stainless Steel 97 40 001 Injection Valve PEEK 77 40 027 Stator Face Assembly 77 50 016 Rotor Seal Injection Valve Vespel
28. ANALYSIS PROGRAM by using the F3 key Five relay functions can be programmed which will activate external functions or pulses With the CURSOR keys the positions for entering the values can be selected The values are entered with the numeric keys or with the SELECT key All time values are relative to the time of injection with the injection of a sample the time counter starts at 0 For the pulse transfer a 15 pin connector is installed at the rear side of the instrument AUX FUNCTION The relays can be programmed for setting defined signals on off or automatic switching after a certain pulse duration entered in the Instrument Configuration Menu act SAMPLE o oy AUXILIARY FUNCTIONS PROG NO 1 FUNCTION ACT OFF PULSE 0 1 3 4 STATUS ANALYSIS EN PRIO PROGRAM SAMPLE Picture 22 Auxiliary Functions Menu DESCRIPTION The Vial List Menu displays the following information in PROG The number of the Analysis Program to be edited i n FUNCTION NO The number of the Output relay Display the actual status the relay 0 OFF 1 n SEC Enter the time when the relay is switched on n OFF SEC Enter the time when the relay is switched off n PULSE Select if this output should use a pulse or a static signal PULSE Signal is switched on for a time period specified the INSTRUMENT CONFIGURATION MENU After this period the relay is Version 3 2 April 2007
29. CE EM PRIO QUIT RESET SAMPLE Picture 13 Function Key Area AANA CONTENT AREA The content area is the area between the status bar and the function key area It shows the actual menu content with text and parameters This is the region where parameter changes can be done Navigating through the content area is done with the CURSOR keys and the screen cursor is updated accordingly Version 3 2 April 2007 Page 28 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler Changing parameters within specific menu is done as outlined below 5 move the screen cursor to the value you want to change by using the CURSOR keys enter the new value by using the numeric keys 0 9 or the SEL_UP and SEL_DOWN keys depending on the kind of value Whenever a value is selected and a is displayed the value can be edited only with the SEL UP and SEL DOWN keys Version 3 2 April 2007 Page 29 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 7 1 MAIN MENU This menu can be displayed at any time by pressing the MENU key at the front panel act 2 gt MATN ENU VER 1 10 15 02 03 STATUS PRIORITY SAMPLE SAMPLE SEQUENCE ANALYSIS PROGRAM WASH PROGRAM INSTRUMENT CONFIGURATION DERIVATIZATION PROGRAM LOCK SAMPLE Picture 14 Main Menu Q 1
30. If cooling heating unit optional is installed the requested temperature can be entered here otherwise NO is displayed Use the SELECT key to define the time scale of the instrument available options are seconds 0 1 i min or 1 min Select the appropriate operation mode here INTERN The instrument is controlled internally by pressing START and STOP EXTERN The instrument is controlled externally via TTL start signal SERIAL instrument is controlled RS 232 serial interface This mode is used when the 5200 is controlled by data system e g ChromStar Here you can enter the duration of the TTL relay pulses like the START or INJECT function Switch to Service Program 1 Menu Switch between English and German language Switch to Service Program 3 Menu Show Priority Sample Menu Page 46 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 7 9 1 SERVICE PROGRAM 1 The service program is displayed by selecting the Instrument Configuration Menu and pressing the Function Key F2 In this program the standard position settings are displayed When using different sample racks the values have to be adjusted in this program For different operation various racks are available s analytical version racks for 120 vials with 1 5 ml volume preparative version racks for 48 vials with 5 ml volume S micro version sliding unit for
31. OPERATION MANUAL Rh ndorfer Strasse 51 S 5200 Autosampler Schambeck SFD GmbH 53604 Bad Honnef 5 1 1 OPERATION PANEL The programming and control of the pump is done by a stepwise dialog using different menus With the Function Keys F1 F5 positioned below the display different menus functions can be selected directly depending on the current menu With the numeric keys values are entered O t 29 0 STOP START Picture 2 Operation Panel 1 Function keys F1 F5 The actual function of the keys is shown on the display These are dependent on the current menu selected 2 MENU key With this key it is possible to select the main menu at any time 3 DELETE Key Deletes the current value 4 SELECT keys For selecting variable settings in the individual menus 5 CURSOR keys For navigating through the display menus 6 STOP key Stop Hold the instrument 7 START key Start the instrument 8 Numeric Keys 0 9 Used for entering numeric values 9 ENTER key Used for entering values Version 3 2 April 2007 Page 13 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 5 2 BACK SIDE VIEW At the rear side of the Autosampler the communication part is installed like the serial communication RS 232C Interface for the operation with a and an additional connection for the remote control of external components Due to these
32. TION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 2 S 5200 Autosampler 1 STANDARD ACCESSORIES 1 piece Drain Tubing Silica 1 piece Bottle for washing solutions volume 500 ml with Teflon tubing and fitting connector 1 piece Bottle for waste volume 1000 ml with Teflon Tubing and fitting connector 2 pieces Standard Sample Racks for 60 x 1 5 ml vials 1 piece Power Cable 100 pieces Sample Vials 1 5 ml or 2 ml 100 pieces Screw Caps with Septum 2 pieces Fittings with ferrules stainless steel or PEEK 2 pieces Capillaries I D 0 25 mm stainless steel or PEEK 1 piece Remote Control cable w Connector 1 set Fuses The accessories enclosed can vary depending on the version of Autosampler ordered 1 1 VERSIONS amp UPGRADE OPTIONS The Autosampler S 5200 is available in 3 different versions and can be upgraded with several options S Fixed Volume Injection Version Standard Version The standard version is delivered with 20 ul sample loop and 500 ul syringe The parts coming into contact with the liquids are made of stainless steel For special application the sample loop and syringe can be exchanged With programmable eluent segment to ensure that the sample segment is transported completely into the sample loop With programmable air segment to keep the eluent and sample segment apart For the injection of larger volumes e g for semi or preparative applications the two sample tacks ca
33. The standard version of the Autosampler S 5200 comes with a sample loop of 100 ul To ensure accurate dosage the syringe sucks on a certain volume of eluent To keep the sample and eluent apart an air segment can be programmed which will be sucked on through the needle Afterwards the sample is sucked on by the stepper motor driven syringe Even small gas bubbles can affect the exact measurement of the sample volume Eluent and wash solution have to be degassed before operation FIX VOLUME INJECTION MODE The sample volume is dependent on the sample loop installed With this method a distinct surplus of sample has to be programmed 1 2 5 times of sample loop volume To reduce the sample loss an eluent segment can be programmed which will be sucked on before the sample segment In order to keep the sample and eluent apart an air segment can be programmed Even small gas bubbles can affect the exact measurement of the sample volume Eluent and wash solution have to be degassed before operation Version 3 2 April 2007 Page 22 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler 6 3 WORKING PRINCIPLE VARIABLE 6 3 1 TAKING THE SAMPLE The sampling unit is moved to the selected sample vial with the help of stepping motors First the programmed eluent volume is sucked from the wash solvent bottle into the syringe 3 2 Way Valve S 52 na
34. URE INDEX Picture 1 Front Side View a a aa rrrsssssssssssssssssssssssssssssssssssssssssssssssssssssssssssssse 12 Picture 2 Operation Panel nant n Q UU e e CQ s 13 Picture 3 Back Side View so sus EE REGE 14 Picture 5 eos LL ua 19 Picture 5 Working Principle Eluent nat 23 Picture 6 Working Principle Air 23 Picture 7 Werking Prineiple Sample xoa ooo eH D e ea 24 Picture 8 Working Principle Transfer to the Sample Loop 25 Picture 9 Working Principle Filling the Sample nennen 25 Picture 10 Picture 11 Picture 12 Picture 13 Picture 14 Picture 15 Picture 16 Picture 17 Picture 18 Picture 19 Picture 20 Picture 21 Picture 22 Picture 23 Picture 24 Picture 25 Picture 26 Picture 27 Picture 28 Picture 29 Picture 30 Picture 31 Picture 32 Picture 33 Working Principle Sample 26 Working Principle Wash Cycle 27 ot el Mutant MOI ORI MIDI 28 28 Main MU lt
35. ample as well as wash solvent is exactly measured and transported by the syringe For certain applications the standard syringe 500 ul can be exchanged by a syringe of different volume max 5000 ul For sampling the needle is moved to the vial lowered down and the programmed sample volume sucked in by the syringe Accurate dosage is possible due to the large amount of steps 17 steps ul with a 500 ul syringe For the following wash cycle the 3 2 way valve switches to the wash solvent and the syringe sucks on the wash solvent After the wash cycle the valve is switching back to the transfer capillary connected to the needle The wash solvent present in the syringe is pushed out and transported through the transfer capillary and needle to the purge port or inject port Important For reliable operation no air bubbles should come into the syringe Should there be any air bubbles present in the syringe they have to be removed through several wash cycles or by flushing with organic solvent Version 3 2 April 2007 Page 20 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 C S 5200 Autosampler 2 6 2 5 WASH SOLVENT BOTTLE For flushing the system before the next injection is carried out a wash cycle program can be selected The 3 2 way valve switches to the wash solvent capillary and the syringe sucks on the volume programmed from the wash solution bottle With most applications the eluent is als
36. aps Pack 100 pieces 70 04 103 Screw Caps w Septum Pack 100 pieces Version 3 2 April 2007 Page 74 74
37. cing the defective part Contact the manufacturer about replacing the defective part f Contact the manufacturer about replacing the defective part f Contact the manufacturer about replacing the defective part f Contact the manufacturer about replacing the defective part f Page 59 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 2 S 5200 Autosampler 10 10 1 ADJUSTMENT OF NEEDLE POSITION In case the needle inject position is not found malfunctioning check first the tension of the driving belts If the defect is not caused by them the needle position has to be adjusted with the help of the SERVICE MENU 10 1 1 MODIFIED SAMPLE RACKS The autosampler comes with two standard sample racks if not otherwise ordered for 120 samples In case special vials of different shape and dimensions as the standard vials have to be used they can be ordered separately The user has to modify only the programming for the sample racks The sample racks are coded and are placed into the sample chamber without any danger of mixing them up The positions of the vials are numbered for the standard rack from 1 to 60 and 61 to 120 The needle has to be programmed via the diagonals between vial no 1 and 60 as well as between vial no 61 and 120 For this the sliding arm has to be moved to these positions SERVICE PROGRAM 2 and the number of steps needed to be entered into t
38. ck in END X X position of the last vial in this rack n END Y Y position of the last vial in this rack n NX Number of vials in X Axis of this rack n NY Number of vials in Y Axis of this rack F1 STATUS return to Status Screen F2 INSTR CONFIG Return to INSTRUMENT CONFIGURATION Menu F3 SERVICE PROG 2 Show SERVICE PROGRAM 2 Menu F5 PRIO SAMPLE Show PRIORITY SAMPLE Menu Version 3 2 April 2007 Page 48 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 7 9 2 SERVICE PROGRAM 2 The service program is displayed by selecting the Service Program 1 and pressing the Function Key F3 Note The program can be only entered if the legitimation code PASS NO was set in the Service Program 1 In this submenu the exact value settings of the needle s position co ordinates can be determined For this the needle is manually moved with the cursor keys to the single positions and the co ordinates displayed have to be documented acr OAMPLE gt SERVICE 2 STEP WIDTH 100 X AXIS STEPS 0 lt 600 Y AXIS STEPS 0 lt Q Z AXIS STEPS 0 lt Q U SYRINGE STEPS Q ACT 0 17250 INJ VALVE 1 2 PUR VALVE 4 5 Q STATUS INSTR SERVICE STEP PRIO CONFIG PROG 1 WIDTH SAMPLE Picture 26 Service Menu 2 keys 1 and 2 press either key and confirm with ENTER The injection valve can then be moved to the selected position by
39. ct position each shaft is controlled by a separate stepping motor All the shafts are moved via linear slideways Version 3 2 April 2007 Page 18 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler 6 2 2 SAMPLING PART The injection system the Autosampler consists of the following six important units Transfer Capillary Dosing Syringe Sample Racks Washing Solution Injection Valve DRAIN COLUMN PUMP Cm 0000000006000 Sample Loop Picture 4 Sampling Part s The Sample Needle mounted to guide bars is stepper motor driven in X Y Z axis The needle is moved to the individual sample vial lowered the septum pierced through and the sample taken The Transfer Capillary between the sample needle and syringe A pre selected sample volume is measured exactly by the syringe and sucked into the capillary The 3 2 Way Valve is positioned above the syringe For sucking on sample volume air segment or wash solvent eluent segment the valve switches automatically The Syringe where the piston is moved up and down with a linear driven stepper motor The selection of the stepping motor s steps ensures the accurate measurement of the volume to be sucked on Version 3 2 April 2007 Page 19 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler S The Wash Solvent the syri
40. d a d HU d P S 37 7 5 Analysis Program MERU u c it tri d i d t d t dH x 38 7 6 Ous au EHE E EN HE 40 T Auxiliary F nctions Mert 2 1 22st ded t d d Hd e Md Hd M S Hd URL EE 41 7 9 Wash Program MerHnU h 43 7 9 Instrument Configuration 22 45 1 91 Service Program Hales ga Sa ss a ha SOD SSS SSD 47 T92 Service Program 2 ce disce ee 49 T93 Service Program d dide uuu 51 8 mmm 52 ex Dervaltisationixample 52 Version 3 2 April 2007 Page 2 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 PL S 5200 Autosampler Menit m 55 Set p Prograimis 2 5 Mees ee ee ee Baas 55 91 4 Analysis iiit aat ia aie to duin dai tee Er eas a c 55 9 1 2 Washi program it iced ie eit i timi t c iut cie iiti i ui Et t 55 9 1 3 Sample Sequencoe a r 56 9 2 Run the Instr rmiemt iet te 56 9 2 1 Starting an analysis sequence nn nnne nnns 56 9 2 2 Stopping the Analysis sss o niit oen ite ea i it n i e c ni i en 56 9 2 3 External
41. e and fitting to the connection DRAIN on the back side SILICA TUBING At the rear side of the instrument a connecting piece for removing the wash solvent when using the PURGE PORT for flushing the needle is installed Slip the Silica tubing onto this connection and position the other and of the tubing into a lower placed water reservoir SAMPLE RACKS Place the sample rack 1 positions 1 60 at the sample chamber s left side and rack 2 61 120 at the right side The pivots mounted to the racks bottom side have to snap into the appropriate fixtures REMOTE CONTROL Please refer to the functions of the 9pin Sub D connector to 10 6 1 Remote Control Version 3 2 April 2007 Page 11 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 5 GENERAL DESCRIPTION 5 1 FRONT SIDE VIEW All parts necessary for the operation are positioned on the front side of the instrument Via the large LCD all functions can be controlled at any time The integrated keyboard makes it possible to program the pump the menu for nearly all analytical applications co 9090 CRORE CLORO STOP START S 5200 Autosampler Picture 1 Front Side View Large Graphical Display Keyboard Sample Chamber w Sample Racks Capillary connections not on Amino Acid Analyzer variant Ron Version 3 2 April 2007 Page 12 74
42. ect YES when you want to wash before each injection n WASH AFTER EACH INJECTION Select YES when you want to wash before each injection WASH AFTER EACH VIAL Select YES when you want to wash after each vial WASH POSITION Select at which position the wash step should be performed You can either select the Injection Port Inj Pos or the default Washing Port Default 4 Version 3 2 April 2007 43 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler FUNCTION KEYS Key Function _ Description F1 STATUS return to Status Screen F5 PRIO SAMPLE Show Priority Sample Menu Version 3 2 April 2007 Page 44 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 7 9 INSTRUMENT CONFIGURATION MENU The instrument configuration program is selected by using the MAIN MENU and key 5 The parameters defined for the operation are displayed and can be adjusted PE DE om er IST CONFIGURATION 29 SYRINGE VOLUME SAMPLE LOOP VOLUME ELUENT SEGMENT SAMPLE COOLING TIME SCALE OPERATION MODE PULSE DURATION STATUS SERVICE DIALOGUE SERVICE PRIO PROG 1 GERMAN PROG 3 SAMPLE Picture 24 Instrument Configuration Menu DESCRIPTION The Instrument Configuration Menu displays the following information aa
43. f the four seal pins using a screwdriver Check if there are any scratches on the rotor s stator s surface A Version 3 2 April 2007 Page 67 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler 10 5 2 REASSEMBLING THE VALVE The new rotor seal has to be placed into the position The rotor seal must be correctly oriented with rotor seal slots facing the stator Reassembly the other part and mount the stator Tighten each of the three screws a little at a time and finally tighten them securely Before using the autosampler for analysis runs the valve must be flushed with the eluent used Version 3 2 April 2007 68 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 10 6 FUNCTION CONNECTORS 10 6 1 REMOTE CONTROL PIN FUNCTION START STOP ERROR N O ERROR N C INJECT N O GND INJECT N C ERROR COM INJECT COM O OQ N 10 6 2 RS 232 SERIAL INTERFACE H z FUNCTION DCD RXD TXD DTR GND DSR RTS CTS RI OMAN O A O N Version 3 2 April 2007 Page 69 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler 10 6 3 AUXILIARY 5 PIN FUNCTION 1 1 2 3 3 4 5 5 9 AUX 1 N C 10 AUX 2 COM 1
44. fixing micro titer plates NOTE If incorrect values are entered the needle can be damaged Before changing the values they should be documented If there are any problems or questions concerning the programming please get in contact with the manufacturer APLE 1 SERVICE 1 PASS NO 123 PURGE X 60s Y 1155 Z 30 0 MM X 605 Y lrl5s Z 30 0 MM SYRINGE VOLUME 500 ul 17250s PRIORITY SAMPLE VIAL NO 120 BEGX ENDX ENDY NX RACK 1 29355 425 494s 055 1 RACK 2 4915 11275 28315 19875 12 STATUS INSTR SERVICE CONFIG 2 SAMPLE Picture 25 Service Menu 1 DESCRIPTION The Service Menu 1 displays the following information ImPASN Enter the legitimation code 123 here n PURGE X Y Z coordinates of the wash port n INJECT X Y Z coordinates of the injection port SYRINGE VOLUME Enter Number of steps for the entire syringe volume default 17250 Version 3 2 April 2007 Page 47 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 S 5200 Autosampler 53604 Bad Honnef n PRIORITY SAMPLE VIAL NO Enter the Vial Position of the priority sample default 120 i n RACK1 This row of coordinates is valid for Rack 1 left n RACK 2 This row of coordinates is valid for Rack 2 right BEG X X position of the first vial in this rack Y position of the first in this ra
45. he SERVICE PROGRAM 1 WARNING For this procedure the autosampler must be connected to the power supply Programming procedure Remove the cover of the autosampler Press the Menu key MAIN MENU Select INSTRUMENT CONFIGURATION 5 Press the function key F2 SERVICE PROGRAM 1 Enter the legitimation code 123 Press key F3 SERVICE PROGRAM 2 The sliding arm moves to the home position Press key F4 STEP WIDTH Select a reasonable step width 1 10 100 500 1000 with the F4 key The coordinate is selected with the CURSOR keys The sliding arm is moved step by step through the SELECT keys Q uh uh With the help of these both keys the sliding arm can be moved along the coordinate requested For the exact positioning a step size of 10 and then finally of 1 is recommended Version 3 2 April 2007 Page 60 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 diee S 5200 Autosampler The arm has to be positioned in such a way that the needle injects exactly in the center of vial 1 60 61 and 120 The x and positions of each vial have to be documented and entered in SERVICE PROGRAM 1 Enter the values in SERVICE PROGRAM 1 for rack no 1 x coordinate of vial 1 at and y coordinate of vial 1 at BEGY x coordinate of vial 60 at ENDX and y coordinate at ENDY and for rack no 2 x coordinate of vial 61 at BEGX and y coordinate of via
46. he wash solvent is then transferred through the needle to the drain port or through the injection unit to the drain Version 3 2 April 2007 Page 26 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 3 2 Way Valve Injection Port a DRAIN COLUMN PUMP Sample Racks Washing Sample Solution Loop Picture 11 Working Principle Wash Cycle Version 3 2 April 2007 Page 27 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler 7 SCREEN MENUS All menu screens have a uniform design and are divided into 3 parts the status bar the function key area and the content area STATUS BAR The status bar is always displayed on the upper part of the screen regardless of which menu is currently active act 2 Picture 12 Status Bar The status bar displays the following information Sample Range SET Current Sample ACT Analysis Time Run Status Error Code FUNCTION KEY AREA The function key area is displayed on the bottom part of the screen This area shows the function of the corresponding key F1 to F5 The actual function of each key depends on the current menu An empty function key area of a specific key denotes no assigned function in the current menu VIAL E SEQUEN
47. l 61 at BEGY x coordinate of vial 120 at ENDX and y coordinate at ENDY The positions for the injection port and purge port are selected as described above and entered in SERVICE MENU 1 Also the SERVICE PROGRAM 1 is used for the setting of the z axis of the inject position The z settings approx 15 0 mm have to be adjusted in very small steps until the needle holder can be pushed downwards by hand only approx 0 5 mm during the injection process The same z coordinates have to be entered for the purge position In SERVICE PROGRAM 2 the functions for the inject port and purge port can be displayed and tested by entering the appropriate function numbers Note Don t put your hand into the sample chamber during operation In case somebody manipulated in the sample chamber during operation and has accidentally touched the needle the needle no longer detects the vial positions and inject port the autosampler has to be switched off immediately and the needle has to be checked for any damage Version 3 2 April 2007 Page 61 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler OOOOO OOOOO OOGOOOODOO Picture 30 Sample Rack Positions Purge Port Injection Port Derivatisation Ports Beginning of Rack 1
48. le dilution mode i e up to three different derivatisation reagents and the wash solution can be automatically added to the sample Each dosage added to the sample Mixing cycle and reaction time is variable The vials with the samples have to be positioned in the right sample rack 61 120 Empty sample vials will be positioned in the left sample rack 1 60 they are used as mixing vials i e each sample vial has a defined mixing vials at the corresponding position The derivatisation vials 5 ml are positioned behind the sample racks Picture 28 Derivatisation Vial Positions 1 2 3 4 5 Derivatisation Vial A Derivatisation Vial B Derivatisation Vial C Mixing Vials Rack Sample Vials Rack 8 1 DERIVATISATION EXAMPLE The following example assumes the following procedure Version 3 2 April 2007 Page 52 74 Schambeck SFD GmbH Rh ndorfer Strasse 51 53604 Bad Honnef OPERATION MANUAL S 5200 Autosampler The use now prepares three 5ml vials with the Reagents A B and C and places them in the Derivatisation Vial places Then he places three empty vials in the left sample rack at positions 1 3 Finally he places his 3 samples in the right sample rack at positions 61 63 The positions of the individual vials are shown on the diagram below OOOOO e9eeoo ooooolooooo OOOQOQO OOOOO OOQOQOQO OOOOO OOOO O00 O OOO 00 O ese e
49. ligence during installation Before putting the instrument into operation read the manual carefully and should there be any further questions please get in contact with your supplier 2 1 GENERAL ELECTRICAL HAZARDS Check actual line voltage to confirm that the set voltage on the rear side voltage selector and fuse carrier of the instrument is correct Before changing the instrument s voltage or before changing defect fuses disconnect the instrument from all power sources The instrument has to be plugged into grounded wall sockets only This instrument can be used only with other instruments which comply with the general safety regulations Connect all cable connections before switching on the instrument 2 2 GENERAL PRECAUTIONS In order to avoid any damages perform periodic leak checks all installed supply lines The instrument is only allowed to be used for applications with specifications described in this manual For flammable and or toxic solvents follow a regulated and approved waste disposal program Never dispose of such products through the municipal sewage system The instrument is suitable for operation between 10 C and 35 C surrounding temperature Through improper handling the needle can be damaged or broken Also please be aware of the danger of injury when putting your hand into the sample chamber during operation ATTENTION Only work in the sample chamber when the instrument i
50. lumn The injection valve remains in this position until the analysis is finished That means that the sample loop is constantly flushed with the eluent Injection Port DRAIN COLUMN Sample Loop Picture 10 Working Principle Sample Injection Switching of the injection valve for transferring the sample to the column With fix volume injection the injection and dosing steps are analogue and the sample overflow will be transported into the waste reservoir 6 3 4 WASHING CYCLE To avoid any transfer of sample material all parts which come in contact with the sample should be flushed after each injection This can be done through the separate needle wash port or via the injection unit If the washing cycle is carried out via the purge port the inside as well as the outside of the needle will be flushed Generally this is not necessary as the sample present at the outside of the needle is sufficiently enough removed through the septum of the vial Only certain special applications need the inside and outside flushing procedure If the washing cycle is done through the injection unit all capillaries which came in contact with the sample are flushed and washed Therefore in most cases the injection unit is selected for carrying out the washing procedure For the washing cycle procedure the syringe used for the sampling is applied The total volume of the needle is filled with wash solvent via the 3 way switching valve T
51. n 69 10 6 1 Remote Control i uuu au uu uuu qq EE EE HU IEEE EU sua teres 69 10 6 2 RS 232 conii die d n EH HR E EE EHE Ganon aes aeons 69 10 6 3 Auxillary FUNCIONS ci dee nun d HE DE IHE EGRE EE EE ERR 70 11 Troubleshootin g e A 71 11 1 Bad reprod cibility SEE RARE GRA RGAE ASA RGA ASA AGAR AS 71 aa EAAUEHIOPET 72 11 3 No Sample Injection can be 72 11 4 72 12 Spare Parts amp Accessories lu wie u J J 73 12 1 Spare Parts s k l Su MN Nu ati e hr eae ae eee 73 122 Sample LOOPS v an Be AR Be wu 73 12 24 PEEK or uu um heh Wel ohhh wh 73 1222 Stainless SIeol 2 coro dore etre e ee eee eh ee a an 73 12 3 Sample 74 Version 3 2 April 2007 Page 3 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler PICT
52. n be exchanged for rack suitable for 5 ml vials For smaller volumes micro titer racks are also available Variable Volume Injection Version The Variable Volume Injection version is delivered with a 100 ul sample loop which can be partially filled Version 3 2 April 2007 Page 5 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler Derivatisation Version Before injection each individual sample can be mixed with up to 3 different reagents A reaction time as well as a washing cycle between the dosage of the single reagents is programmable Chemically Inert Option For aggressive samples or especially with sensitive substances the biocompatible S 5200 PEEK version is recommended All components which come into contact with the sample and or eluent e g sample needle valve and capillaries are made of Polyetheretherketone PEEK Heating Cooling Option For storage of unstable samples the Autosampler S 5200 can be upgraded with a cooling heating device The sample racks can be cooled heated very accurately between 5 and 70 C with built in Peltier elements Version 3 2 April 2007 Page 6 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler 2 SAFETY INSTRUCTIONS The manufacturer does not warrant for any defects or damage resulting from incorrect operation and maintenance non observance of the manual s instructions and neg
53. nge sucks a programmed volume of wash solvent for flushing the syringe and the transfer capillary The wash solvent is pushed into the inject port via the sample needle The sample valve with the sample loop where the sample is injected into the system and transported together with the eluent to the separation column 2 6 2 1 SAMPLE NEEDLE The needle is mounted to a sliding carriage and is moved through step motors in X Y direction When the needle is directly above the selected sample vial it will be lowered down Z direction This is done by lowering the sliding carriage where the needle is mounted to The needle pierces through the septum The sample is sucked into the transfer capillary between needle and stepper motor driven syringe However if no vial was placed into the selected vial position the vial sensor plate activates an optical sensor The exact vial position error will be displayed 2 6 2 2 TRANSFER CAPILLARY The transfer capillary has a certain length and diameter This ensures that the sample remains in the capillary only and will not be sucked into the syringe For flushing the system only the capillary and the needle has to be flushed not the syringe 2 6 2 3 3 2 WAY SWITCHING VALVE The switching valve is mounted on top of the syringe Depending on the switching position sample air segment is sucked into the transfer capillary or wash solvent eluent segment is sucked into the syringe 2 6 2 4 SYRINGE S
54. o used as washing solution 2 6 2 6 SAMPLE VALVE For transporting the sample into the eluent stream a motor driven 6 position injection valve is used With this valve the sample is injected in the sample loop and together with the eluent stream transported to the separation column With the fixed volume injection method the installed sample loop is overfilled with the sample refer to above drawing pos 1 and pos 4 With variable volume injection mode an oversized sample loop is partially filled with the sample volume selected Turning of the valve s rotor will switch the sample loop into the eluent stream and the sample volume is transported together with the eluent to the column When the sample loop is to be filled the rotor of the 6 way switching valve is switching to S Port 1 and 6 Connecting inject port and sample loop S Port 4 and 5 Connecting sample loop with the drain S Port 2 and 3 Direct connection of HPLC pump to the column For the injection of the sample the valve is switched Now the eluent is directly transported through the sample loop The sample dosed via the sample loop is transported together with the eluent stream to the column Hereby the rotor switches to S Port 3 and 4 The HPLC pump is connected to the sample loop S Port 1 and 2 The end exit side of the sample loop is directly connected to the column S Port 5 and 6 connected The sampling procedure is followed up by the flushing cycle Hereby the
55. ons to be performed for each vial WASH PROGRAM Enter the number of the wash program to be used with this analysis program in SYRINGE SPEED Here you can select a different speed for the syringe i movement Besides the default value of 50 you can select 100 and 33 Version 3 2 April 2007 Page 38 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 2 S 5200 Autosampler NEEDLE This value specifies the depth of the injection needle I movement This value have to be adjusted to specific vials e g Eppendorf vials use Needle Depth of 39 in ANALYSIS TIME This is the runtime for this analysis program The next sample injection will start after this time has elapsed SAMPLE TEMPERATURE Here you can enter the temperature of the sample racks Note that this feature is only available with the cooling option AIR SEGMENT Here you can enter the size of the air segment between the taken sample and the eluent This feature prevents the mixture of eluent and sample which leads to an inaccurate sample injection NOTES If you control the S 5200 Autosampler via RS 232 Analysis Program 1 will be used Make sure that all parameters of program 1 are valid for your method D m F1 STATUS return to Status Screen F2 VOLUME MODE Switch between fix and variable volume mode Note that the variable volume mode is only available with the variable volume
56. operation WE COPIE 34 sm STATIS 7 SAMPLE TEMP SEQUENCE NO INJECTION NO ANALYSIS PROGRAM WASH PROGRAM WAIT VIAL EROROR 0 TOTAL SAMPLE VOL Q u 1 1 lt VIAL E SEQUENCE ws PRIO QUIT RESET SAMPLE Picture 17 Status Screen DESCRIPTION The STATUS SCREEN displays the following information SAMPLE TEMP If the cooling option is available this field shows the current sample temperature SEQUENCE This field displays the current sample sequence INJECTION This field shows the Current Injection and the total number of injections for the current vial n TOTAL VOL This field shows the total sample volume taken by the instrument ANALYSIS PROGRAM Here you can see the number of the Analysis Program used for the current sample WASH PROGRAM This field displays the number of the used Wash Program n WAIT In this field you can see the Wait Time countdown if you have selected Wait Time the Instrument Configuration Menu VIAL ERROR In case of an Vial Error this field displays row of numbers each the vial number where an Vial Error occurred You can delete each single entry by pressing the F2 key This is Version 3 2 April 2007 Page 34 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 S 5200 Autosampler 53604 Bad Honnef necessary to restart a sequence as the instrument cannot
57. pressing the SEL UP or SEL DOWN key DESCRIPTION The Service Menu 2 displays the following information n STEP WIDTH Display of the currently selected step width This is the amount of step by which the selected axis will moved X AXIS STEPS Current position in steps of the X Axis Y AXIS STEPS Current position steps of the 5 Z AXIS STEPS Current position in steps of the Z Axis MX number of steps possible for this axis SYRINGE STEPS Current position in steps of the Syringe Axis INJ VALVE You can manually move the injection valve with the Version 3 2 April 2007 49 74 OPERATION MANUAL Rh ndorfer Strasse 51 2 S 5200 Autosampler Schambeck SFD GmbH in PURGE VALVE You can manually move the purge valve with the keys 4 and 5 press either key and confirm with ENTER The injection valve can then be moved to the selected position by pressing the SEL UP SEL_DOWN key Lu ii iii iii i Mf n np FUNCTION KEYS 2 ao INSTR CONFIG Return to INSTRUMENT CONFIGURATION Menu SERVICE PROG 1 Show SERVICE PROGRAM 1 Menu STEP WIDTH The step width for the axis movement can be set with this key PRIO SAMPLE Show PRIORITY SAMPLE Menu Version 3 2 April 2007 Page 50 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH
58. s not in operation For trouble free and reliable operation it is recommended to use only filtrated 0 45 um or particle free samples for the degassing process Version 3 2 April 2007 Page 7 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler standard model 5 5200 comes with a needle of stainless steel To avoid corrosion the ph value of the sample should be between 2 and 11 Chemically inert version the needle is optionally available The wash solution and eluent used for the analysis have to be degassed before operation The instrument should be cleaned only with appropriate cleaning agents Version 3 2 April 2007 Page 8 74 Schambeck SFD GmbH Rh ndorfer Strasse 51 53604 Bad Honnef OPERATION MANUAL S 5200 Autosampler 3 TECHNICAL SPECIFICATIONS Sampling Control Dialogue Communication Sample Loop Sample Dosage Material Reproducibility Memory Effect Washing Program Analysis Time Sample Racks Power Requirement Fuses Working Temperature Dimensions Weight Version 3 2 April 2007 X Y Z Operation stepper motor driven syringe integrated microprocessor Motorola 68000 selectable between English and German RS 232 interface and interface for system control remote control 5 integrated REED relays inject marker and or remote control of external components exchangeable standard volume 20 ul other volumes
59. s to be completely degassed before operation Even smallest gas bubbles especially with very low sample volumes can cause incorrect dosage thus causing poor reproducibility of the analysis results SILICA CAPILLARY The silica capillary with the inside diameter of approx 5 mm must be slipped onto the connection DRAIN 3 and 4 The end of the capillary should end in a lower placed drain reservoir DRAIN This drain is used for removing not needed samples and washing solution during flushed loop injection method The Teflon capillary has to be fitted with the fitting and the ferrule to the connection 7 and has to lead into the waste bottle 1000 ml positioned at the same height as the instrument The waste bottle has to be emptied before the fluid level is even with the flow capillary 5 4 CABLE CONNECTIONS INTEGRATION INTO AN ANALYSIS SYSTEM The Autosampler is integrated into the system via the RS 232 interface or D Sub connector REMOTE CONTROL and can be controlled via contact closures Information like error messages or injections performed can be detected at the output connector Following functions are possible Start of sample sequence End of sample sequence Error message Message about the injection performed Version 3 2 April 2007 Page 15 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler REMOTE CONTROL OF EXTERNAL 5 In case
60. sample needle and the injection valve are flushed with wash solvent to avoid any transfer of sample remaining 2 6 2 7 FIX VOLUME INJECTION VARIABLE INJECTION MODE The Autosampler S 5200 with variable injection mode can be used also for fix volume injection mode Fix volume injection The sample volume is dependent on the size of the sample loop which will be overfilled with sample Turning of the valve s rotor will switch the sample loop into the eluent stream and the sample volume is transported together with the eluent to the column Hereby unique accuracy and reproducibility is achieved The disadvantage of this method the sample loop has to be changed when injecting different sample volumes Also there will be a loss of sample substance caused by the overfilling of the sample loop Version 3 2 April 2007 Page 21 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 sn S 5200 Autosampler Variable volume injection The measurement of the sample volume is done by the syringe The sample segment is transferred into an oversized sample loop partially filled Due to the high resolution of the syringe s stepper motor 17 steps ul with a 500 ul syringe precise dosage and good reproducibility of the analysis results is possible with this operation method The loss of sample substance can be neglected due to the accurate syringe dosage and the programmable eluent air segment VARIABLE INJECTION MODE
61. sed for the Priority Sample PRIORITY SAMPLE In this field you can see if the Priority Sample is Inactive or Active The information is also displayed in the Status Bar right next to SAMPLE FUNCTION KEYS 1 STATUS return to Status Screen 4 ABORT PRIO S Abort the Priority Sample Run Version 3 2 April 2007 Page 36 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 7 4 SEQUENCE MENU From the Main Menu and 2 the sample sequence screen is selected This screen combines the samples vial from to with the analysis program SAMPLE SEQUENCE 1 4 T0 1 ta Co 10 10 10 q E L co Picture 19 Sample Sequence Menu DESCRIPTION The Sample Sequence Menu displays the following information FROM Enter the first vial ofthe sequence step in TO Enter the last vial of the sequence step PROG Enter the Number of the Analysis Program to used for this sequence step
62. sitioning Sensor Valve Positioning Drive Valve Slide Syringe Spindle Driving Shaft Syringe Motor Positioning Sensor Syringe Forked Support Sliding Carriage Knurled Fitting Plate Spring O O AN O QO WN a Picture 31 Syringe Schematic Version 3 2 April 2007 Page 63 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 10 3 REPLACING THE INJECTION NEEDLE Should the injection needle been damaged or in case the needle gets caught in the top of the sample vial the autosampler has to be switched off Check the tip of the needle concerning fine edges etc if necessary exchange the needle Shaft Driving Belt Belt Connection Injection Needle Injection Needle Fitting Air Needle Screw Top Part Air Needle Bottom Part Vial Sensor Plate Vial Sensor Vial Stripping Stop O QO GQ N e Picture 32 Needle Schematics S After finishing the flushing cycle turn off the autosampler and disconnect the power supply S Remove the top cover of the instrument and the covering of the sliding carriage The needle is fixed by a tension screw positioned at the angle s lead in hole The angle is mounted with 4 screws to the sliding carriage moving up and down through a driving belt S Atthe upper part of the needle the fitting with the capillary has to be removed Use the pliers to unscrew the needle insert Then the needle
63. tarting the sequence press F3 SEQUENCE RESET In case of any error messages these have to be deleted with the STOP or F2 Vial Error key S checkthe operation mode INTERN EXTERN Adjustments can be done in the CONFIGURATION MENU 5 press the START key during the sample processing changes can be done to all the submenus which will be activated in the next injection 9 2 2 STOPPING THE ANALYSIS In case an error was made e g mistake in filling the vial which is detected after the analysis has been started the analysis process can be stopped by pressing the STOP key This will stop the current time counter the functions however will remain activated In the top right Version 3 2 April 2007 Page 56 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler corner HOLD displayed Now the be placed the correct position after pressing the START key the operation is activated again In case a serious problem appears and the analysis sequence should be totally stopped the STOP key has to be pressed once again Select in the MAIN MENU the STATUS display and by pressing F3 SEQUENCE RESET the sequence will start again with the first sample The START key has to be pushed to start the processing 9 2 3 EXTERNAL CONTROL press the MENU key move the cursor to the INSTRUMENT CONFIGURATION MENU and press ENTER
64. the AIR SEGMENT field and enter a suitable value recommended value 3 yl all entered values are stored under the given program no 9 1 2 WASH PROGRAM S S press MENU key move the cursor to the WASH PROGRAM MENU and press ENTER or directly enter the menu with the 4 key Version 3 2 April 2007 Page 55 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 2 S 5200 Autosampler with cursor to enter the program under which this program should stored recommendation for standard operations 100 syringe speed 1 wash step wash after each injection wash position inj pos S all entered values are stored under the given program no 9 1 3 SAMPLE SEQUENCE press MENU key move the cursor to the SAMPLE SEQUENCE MENU and press ENTER or directly enter the menu with key 2 5 move the cursor to the FROM field and enter the number of the first vial of the sequence e g 1 S move the cursor to the TO field and enter the number of the last vial of the sequence e g 10 S Move the cursor to the PROG field and enter the number of the analysis program to be used for this sequence e g 3 for the number of the analysis program you ve prepared above 9 2 RUN THE INSTRUMENT 9 2 1 STARTING AN ANALYSIS SEQUENCE 5 check the sample racks positioned correctly and if the vials are placed correctly and filled with sample press the STATUS key before s
65. the Vial Sequence is in the wrong Rack The Rack sizes entered in the Service Menu are different An error was detected with the movement of the Injection Valve An error was detected with the movement of the 3 Way Valve An error was detected with the movement of the X Axis stepping motor An error was detected with the movement of the stepping motor An error was detected with the movement of the Z Axis stepping motor An error was detected with the movement of the syringe stepping Solution Check the injection volume and the Eluent Segment s volume The total volume used for the run must not exceed the volume of the syringe If that doesn t solve this error contact the manufacturer for further help Check the sample rack and make sure that a vialis _ placed in the specified position and clear the vial error before continuing see below Check the Sample Sequence that all sequence steps in use have a FROM TO and PROG value gt 0 Also check that the FROM value is smaller or equal to the TO value i Check the Sample Sequence that they are on the right Rack Pos 61 120 only The left Rack Pos 1 60 is used for the mixing vials u Check the Rack sizes in the Service Menu Both Rack 1 and Rack 2 must have the same number of vials in the X and Y Axis oe Se defective part Version 3 2 April 2007 Contact the manufacturer about repla
66. the autosampler is integrated into a system without any PC the autosampler can be used for the control of the other components Five potential free relay contacts can be programmed in a separate sub menu AUX FUNCTION Menu As control signal the relay uses a time controlled signal or a programmed impulse Load of the relay when controlling external instruments Max Voltage 175 V Max Power 3 0 W Max Current 0 25A CONTROL VIA RS 232 INTERFACE With the help of the RS 232 interface 3 the autosampler can communicate with a PC The RS 232 connector has to be cabled with the RS 232 connector of the PC For starting the data acquisition the inject signal Remote connector has to be connected as a digital signal to the start input of the PC Version 3 2 April 2007 Page 16 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 2 S 5200 Autosampler 6 INSTRUMENT DESCRIPTION 6 1 GENERAL The Autosampler S 5200 is an automatic sample processing system the standard model can inject up to 120 samples The instrument can be used as a stand alone system and can be also integrated into a system controlled via PC The analysis program can be easily adjusted to the individual application through the different menus With the fixed volume injection version the sample volume is dependent on the built in sample loop which is easily exchangeable With the variable injection version the stepper motor driven syringe
67. tting it close the cover Before any transportation of the instrument mount the safety catch again to avoid damage to the instrument 4 3 INSTALLATION NOTE When using the Autosampler S 5200 with the Amino Acid Analyzer S 433 please refer to the Amino Acid Analyzer Installation Manual ELUENT CAPILLARY Connect the eluent capillary stainless steel or PEEK with the appropriate fittings and ferrules to the connection PUMP positioned at the front panel of the instrument The other end of the capillary has to be connected to the pressure side of the pump head SAMPLE CAPILLARY Connect the sample capillary to the connection COLUMN on the front panel of the instrument RACK FOR WASH SOLUTION Install the rack enclosed with the pre mounted screws at the rear panel of the instrument Version 3 2 April 2007 Page 10 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler WASHING SOLUTION Fill the 500 bottle with completely degassed washing solution Place it the appropriate rack on the backside of the instrument and close the bottle Connect the Teflon tubing to the backside connector WASH SOLUTION below the bottle rack BOTTLE WASTE The 1000 ml bottle is used for collecting the waste It has to be positioned on the same level as the autosampler to ensure trouble free transportation into the waste bottle The tubing has to be connected with the ferrul
68. wered into this port Hereby the needle is hermetically sealed through a PTFE seal Via the syringe the sample is pushed into the injection port till the injection valve The eluent and air segment sucked in before remains in the capillary between the injection port and the injection valve The volume of this capillary is approx 28 ul Now the injection valve is switched to the load position and the programmed sample volume e g 20 ul is injected into the sample loop This way no wash solution or air can enter the sample loop The air and eluent segment can be programmed in the analysis menu 3 2 Way Injection Valve Port Pd 1 Sample Eluent Segment Air Segment DRAIN COLUMN i Sample Racks Washing Solution Picture 8 Working Principle Transfer to the Sample Loop Injection Port Eluent Segment Air segment S DRAIN Sample COLUMN PUMP Picture 9 Working Principle Filling the Sample Loop Version 3 2 April 2007 Page 25 74 OPERATION MANUAL Rh ndorfer Strasse 51 5 S 5200 Autosampler Schambeck SFD GmbH 6 3 3 INJECTION After the sample loop filling process is finished the rotor of the injection valve is switched 60 turn and the sample loop with the HPLC pump separation column connected The eluent is now directly transported through the sample loop and flushes the sample loop volume to the separation co
69. x volume injection method an appropriate sample loop has to be installed On request the instrument can be upgraded for other applications S Pre column derivatisation up to three independent reagents can be added to each sample mixed with the sample and programmed with independent reaction times In addition the sample can be diluted up to 1 100 before injection For temperature sensitive samples the sample tray can be cooled or heated with an optional cooling system The heating cooling process is done via built in Peltier elements S For chemical inert operation the instruments parts like needle capillary valve unit etc are made of PEEK and FEP materials Version 3 2 April 2007 Page 17 74 OPERATION MANUAL Schambeck SFD GmbH Rh ndorfer Strasse 51 5 S 5200 Autosampler s Awide range of sample racks for different sample vials can be used Racks from 1 ul up to 5000 ul or micro titer plates are available 6 2 SYSTEM DESCRIPTION 6 2 1 MECHANICS All parts of the instrument cover sample racks sample needle etc which may come in contact with aggressive substances are made of stainless steel and other resistant materials For certain applications e g lon Chromatography where extremely strong acids or concentrated saline solutions are used as eluent the sampling part is made in PEEK The sampling process is done with a stepper motor driven sample needle X Y Z axis For the exact needle inje

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