s 9425 hplc pump system user manual
Contents
1. S 9425 HPLC PUMP SYSTEM AA WARNING Make sure that the eluent bottles are on a higher level than the pump so that the solvents can freely flow downwards 22 4 2 2 Quaternary Gradient Version The following list describes all necessary steps to make the proper capillary connections for the Quaternary Gradient Version Connect the 1 8 PVDF tubings to the eluent inlets A B C and D 2 A 1 8 PVDF capillary is connected between the Gradient Mixing Outlet 3 and the Pumphead Inlet 4 Fix the 1 8 capillaries with the Capillary Holder 1 e Connect a 1 16 capillary Micro Analytical I D 0 5mm Semi Preparatibe I D 0 75mm to the Purge Valve Outlet 5 this capil lary is connected to the autosampler or manual injection valve i 5 9425 HPLC PUMP SYSTEM 5 Element 5 Purge Valve Outlet Make sure that the eluent bottles are on a higher level than the pump so AR WARNING that the solvents can freely flow downwards 23 4 3 Backside Connections 4 3 1 Drain Gas Exhaust Connections The Drain Outlet is only connected in the Quaternary Gradient version while the Gas Outlet is only available with the optional Vacuum Degaser e Connect the supplied gas tubing blue colored to the GAS OUT connector on the backside of the instrument A STOP When working with aggressive and or toxic solvents make sure that any fumes from the GAS OUT connector is properly dis2. MAINS 50 60 Hz POWER 100 240 V FUSE 2 0 AT o q e S N DRAIN 9 8S1 S8t Su 2 54 1LOWIA OU Element 1 Gradient Mixer Module Drain optional 2 Vacuum Degasser Gas Outlet optional 3 4 Power Switch RS 485 Interface Connectors USB Interface Connector 15 3 2 Isocratic Version Description Element 16 3 2 1 Isocratic Version Front Elements The Isocratic Version of the 5 9425 HPLC Pump System has all important parts directly accessible from the front panel when the Front Cover is opened or removed The Capillary Holder 3 holds the pump inlet capillary in place The Pumphead 4 is completely accessible from the front to make capillary connections or change pump sealings The Purge Valve 5 is used for the priming of the pump and also has the pump outlet connection 989 a e PURGE aig B 5 9425 HPLC PUMP SYSTEM 3 2 2 Isocratic Version Functional Elements All functional elements of the 5 9425 HPLC Pump System are located inside the instrument The Display PCB 1 controls the TFT Display and Keyboard It is acces sible when the display panel is removed The Controlled PCB 2 controls the whole pump The Power Supply Unit 3 supplies 24V to the PCB s and pump motor The input voltage is variable from 90 V to 240 V The Pump Mechanic 4 drives the pumphead and
3. B 2 Environmental Conditions B 2 1 Operational Conditions Ambient Temperature ORCOS Ambient Relative Humidity 20 to 80 RH non condensing B 2 2 Storage Conditions Ambient Temperature 20 C to 60 C Ambient Relative Humidity 20 to 80 RH non condensing 50 APPENDIX C ACCESSORIES C 1 Standard Accessories The S 9425 HPLC Pump System is delivered with the following standard accessories Isocratic Version 1 Power Cord EU Type 1 Serial Cable RS 232 e 1 1 8 Capillary FEP 2 m 1 1 8 Fitting amp Ferrule PVDF e 1 1 16 Capillary 0 50mm 60 cm SS or PEEK 1x Wrench 12 x 13mm 1 Wrench 1 4 x 5 16 1x Allen Wrench 2 5mm 1x Allen Wrench 3 0mm e 1x Plastic Syringe w Tubing Adapter e Ix Operation Manual this e 2x Fuse 2 A Gradient Version e 1 Power Cord EU Type 1 Serial Cable RS 232 e 4x 1 8 Capillary FEP 2 e 4x 1 8 Fitting amp Ferrule PVDF e Ix 1 16 Capillary 0 50mm 60 cm SS or PEEK 1x Wrench 12 x 13mm e Ix Wrench 1 4 x 5 16 51 e 1x Plastic Syringe w Tubing Adapter e 1 Operation Manual this e 2x Fuse 2A 52 APPENDIX D VERSION CONTE D 1 Version History The 5 9425 HPLC Pump System Operation Manual is subject to version con trol The version history is continued and noted on every document The access to the original document is restricted to the creati
4. 63 0 3 x 0 68 0 83 For other solvents with an unknown factor an average factor of 0 700 can be used The difference from the correct delivery rate won t be higher than 5 If this accuracy is good enough a medium factor of 0 700 for all or ganic solvents and 1 000 for water can be used APPENDIX B SPECIFICATIONS B 1 Technical Specifications B 1 1 Vacuum Chamber optional of Channels Degassing Technique Wetted Materials Volume per Channel Inner Diameter Capillary Degassing Efficiency 1 2 3 or 4 Applied vacuum through semiperme able membrane Teflon Stainless Steel PEEK lt 500 ul 1 1mm lt 20 dissolved gases remaining in water at 1 0 ml min B 1 2 Vacuum Pump optional Mechanism Stepper Motor driven membrane pump Wetted Material Fumes only Teflon Aluminium EPDM B 1 3 Pump Wetted Materials Flow Rate Flow Accuracy Flow Precision Gradient Mixing Pressure Range Pressure Pulsation Dimensions Weight Power Supply Stainless Steel PEEK PVDF Ceramics Ruby Micro 0 001 4 000 ml min Analytical 0 001 10 000 ml min Semi Preparative 0 001 40 000 ml min 1 0 E 1 000 ml min 0 1 96 RSD 1 000 ml min Dynamic 516 923 ul adjustable mixing volume 0 40 MPa 0 6000 PSI typical 0 1 MPa or 1 0 96 310x165 x 478 mm W x Hx D 7 0 kg 100 250 V 47 63 Hz 20 W depending on material option 49
5. Software Mainb The Software Display is the installed firmware version of the Controller PCB 24V Voltage The 24V Voltage is an actual voltage reading for one of the PCB s controlled voltages Runtime The runtime shows the total runtime of the pump 35 36 6 INSTRUMENT OPERATION 6 1 Overview The S 9425 HPLC Pump System can be operated in 3 different Operation Modes Internal External or Serial 6 1 1 Internal Mode In Internal Mode the instrument is controlled manually with the Keyboard 6 1 2 External Mode In External Mode the instrument is controlled via the Remote Digital I O contacts 6 1 3 Serial Mode In Serial Mode the instrument is controlled by a PC software e g Clarity via RS 232 serial line 6 2 Priming the Pump Before the S 9425 HPLC Pump System can be operated it must be primed with the required mobile phase 6 2 1 Isocratic connect the plastic syringe to the purge valve outlet suck the eluent through the tubing till it starts filling the syringe keep the syringe on the purge valve outlet e press PURGE and check if the syringe is filling with constant speed Now the pump is primed and ready for operation 37 6 2 2 Gradient connect the plastic syringe to the purge valve outlet select the channel A B or D you want to prime with the cursor keys LEFT and RIGHT in the Status Screen open the selected channel with the UP ke
6. includes the camshaft lubrication chamber driving pistons and the stepper motor Element 17 3 3 Quaternary Gradient Version Description Element s 18 3 3 1 Quaternary Gradient Version Front Elements The Quaternary Gradient Version of the 5 9425 HPLC Pump System has all important parts directly accessible from the front panel when the Front Cover is opened or removed The Capillary Holder 3 holds the pump inlet capillary in place The Solvent Inlets Block 4 has an inlet connection for each of the 4 sol vents B C and D and also a connection capillary to the Pumphead s inlet The Pumphead 5 is completely accessible from the front to make capillary connections or change pump sealings The Purge Valve 6 is used for the priming of the pump and also has the pump outlet connection 989 5 e PURGE aig o S 9425 HPLC PUMP SYSTEM 3 3 2 Quaternary Gradient Version Functional Elements All functional elements of the 5 9425 HPLC Pump System are located inside the instrument The Display PCB 1 controls the TFT Display and Keyboard It is acces sible when the display panel is removed The Controlled PCB 2 controls the whole pump The Power Supply Unit 3 supplies 24V to the PCB s and pump motor The input voltage is variable from 90 V to 240 V The Vacuum Pump 4 is mounted on a drain tray It is conn
7. m 000300 u ww Nn N mM m vovN vv ON Nn N w wuwu N So 5 3 6 Submenu Systemmenu 6 Instrument Operation 6 1 Overview 6 1 1 Internal Mode 6 1 2 External Mode 6 1 3 Serial Mode 6 2 Priming the Pump 6 2 1 Isocratic 6 2 2 Gradient 6 3 Operating the Pump in Isocratic Mode 6 3 1 Starting the Pump 6 3 2 Stopping the Pump 6 4 Operating the Pump in Gradient Mode 6 4 1 Starting the Pump 6 4 2 Stopping the Pump 7 Instrument Maintenance 7 1 Pumphead 7 1 1 Pumphead Assembly 7 1 2 Piston Backflushing 7 1 3 Change of Piston Ring 7 14 Replacing Check Valves Appendix A Compressibility Appendix B Specifications B 1 Technical Specifications B 1 1 Vacuum Chamber optional B 1 2 Vacuum Pump optional B 1 3 Pump B 2 Environmental Conditions B 2 1 Operational Conditions B 2 2 Storage Conditions Appendix C Accessories C 1 Standard Accessories Isocratic Version Gradient Version Appendix D Version Control D 1 Version History 34 35 37 37 37 37 37 37 37 38 39 39 39 40 40 41 43 43 43 44 44 44 47 49 49 49 49 49 50 50 50 51 51 51 51 53 53 1 INTRODUCTION 1 1 How to Use this Manual This manual is designed as a reference to the installation operation and maintenance of the S 9425 HPLC Pump System It is strongly recommended to review this manual before operating the in strument The content o
8. mixing chamber are high performance valves to achieve very fast and constant switching times This fast and reliable response of these valves are important for accurate and precise gradient mixing The solenoid valves hold a system pressure of up to 5 bars which enables the use of gas pressure to be applied to the solvent reservoir bottles without any negative effect on the gradient mixing Vacuum Pump Optional The optional online vacuum degasser consists of a Vacuum Pump and four Vacuum Chambers The Vacuum Pump is a high efficiency membrane pump using an advanced Teflon membrane for highest possible chemical compatibility and long lifetime The specific Teflon membrane is devel oped for high frequency deformations to achieve an excellent lifetime of the membrane as chances of ruptures are much reduced Vacuum Chambers The four Vacuum Chambers used in the Quaternary Gradient Module are low volume high efficiency chambers using the advanced Teflon Vacuum Pump Vacuum Chambers The Quaternary Gradient Module The Quaternary Gradient 8 features an integrated vacuum ES 4 vacuum chambers are fitted with pump for online degassing The Y IL high efficiency Teflon AF tub advanced Teflon membrane guaran mro Zara ON ings for low volume and increased tees a long lifetime and maximum 9 A PENO degassing efficiency chemical compatibility De Active Mixer Secure Assembly The Quaternary Gradient Module The Quate
9. the START key The pump will run at the selected flow rate Flow Start Ramp If a time is set for the Start Ramp the flow rate will slowly increase from 0 to the selected flow rate over a selected time e g Start Ramp time This feature gently increases flow and therefore pressure and may increase the lifetime of some specific columns Mode Intern Status HOLD Mode Intern Status Run Prog After the pump reached its flow rate it automatically goes to HOLD this means the pump is running but the gradient program time is on hold The pump will switch from HOLD to RUN after pressing the START key again or by external signal The current state of the gradient program can be checked on the Status Screen be pressing the STATUS key Mode Intern Status Run Prog Mode Intern Status Run Prog Flow 1 0004 Pres 32bar The bottom line shows the current gradient composition while the center of the status screen shows the current step step time and total time 6 4 2 Stopping the Pump The S 9425 HPLC Pump System can be stopped by pressing the STOP key The pump will stop immediately unless a Stop Ramp is set Flow Stop Ramp If a time is set for the Stop Ramp the flow rate will slowly decrease from the selected flow rate to 0 over a selected time e g Stop Ramp time Maximum Pressure In case the Maximum Pressure threshold is met the pump stops immedi ately Minimum Pressure In case the Minimum Pre
10. Bar MPA and PSI All pressure values are shown in this selected pressure units Compressibility The Compressibility can be changed here A Compressibility of 1 000 is used for water and 0 700 for Methanol 5 3 2 Submenu Pump Menu gt Parameters Hold Timeout The Hold Timeout specifies a timeout after which the pump automatically stops when it is currently in Hold If the Timout is set to 0 this feature is disabled Delay Time The Delay Time specifies a delay between starting the pump and the pump actually starting Start Ramp The Start Ramp defines a time in which the flow slowly ramps up when started Stop Ramp The Stop Ramp defines a time in which the flow slowly ramps down when stopped 31 32 5 3 3 Submenu Pump Menu gt Calibration Network Address The Network address can be any number between 0 and 15 It is used for specific cases of external control mode Head The Head settings defines the installed pump head Head Constant The Head Constant is a setting for an individual pump s flow rate adjust ment Do not change this value Pressure Comp The Pressure Compensation is a setting for an individual pump s pressure compensation adjustment Do not change this value Pressure Zero The Pressure Zero is an offset for the installed pressure sensor Only change this value when the pressure sensor is changed 5 3 4 Submenu Gradient Menu Prog Run Sele
11. RN input contact must be closed for external operation Inject Input Connection for a manual injection valve The pump transfer the injection signal to the data system via RS 232 Error Output In case of a pump error this output is set REMOTE Pin Function afo KC 5 INSTRUMENT MENUS 5 1 Keyboard The S 9425 HPLC Pump System parameters can be adjusted at any time via the screen menu and keyboard on the front panel omneo Cw C lae MENU Key With the MENU key you can access the Main Menu and select a sub menu PURGE STATUS Key With the STATUS key you can access the status screen from any menu EDIT Key Use the EDIT key to change any parameters When you press the EDIT key the selected parameter can be changed Confirm the new setting by pressing the EDIT key again CANCEL Key With the CANCEL key you can abort the change of a parameter When pressing CANCEL key instead of EDIT key when changing a param eter the change is discarded and the original value is used CURSOR Keys The 4 arrow CURSOR keys are used to navigate the menus START Key The START key starts the pump 27 5 The STOP key stops the pump PURGE Key The PURGE key START and STOP together is used to purge the pump Make sure that you open the Purge Valve before pressing the PURGE key When activated the Purge will run the p
12. S 9425 HPLC PUMP SYSTEM ISOCRATIC amp QUATERNARY GRADIENT VERSIONS USER MANUAL 5 9425 HPLC PUMP SYSTEM VERSION 1 0 2012 10 25 TABLE OF CONTENTS 5 3 5 Submenu Degaser Settings Contents 1 Introduction 1 1 How to Use this Manual 1 1 1 Symbols 1 2 Safety Information 1 2 General Safety Information 12 2 Intended Purpose 12 3 Environmental Safety 1 24 Electrical Safety 2 Instrument Overview 2 1 General Instrument Overview 2 1 1 Pump Mechanic 2 1 2 Quaternary Gradient Module 3 Instrument Description 3 1 General Instrument Description 3 1 1 Front Panel Description 3 1 2 Back Panel Description 3 2 Isocratic Version Description 3 2 1 Isocratic Version Front Elements 3 2 2 Isocratic Version Functional Elements 3 3 Quaternary Gradient Version Description 3 3 1 Quaternary Gradient Version Front Elements 3 3 2 Quaternary Gradient Version Functional Elements 4 Instrument Setup 41 Unpacking 4 2 Capillary Connections 4 2 1 Isocratic Version 4 2 2 Quaternary Gradient Version 4 3 Backside Connections 4 3 1 Drain Gas Exhaust Connections 4 3 2 Electrical Connections 4 3 3 Remote Connector 5 Instrument Menus 5 1 Keyboard 5 2 Status Screen 5 3 Menu Description 5 3 1 Submenu Pump Menu gt Pump Settings 5 3 2 Submenu Pump Menu gt Run Parameters 5 3 3 Submenu Pump Menu Calibration 5 3 4 Submenu Gradient Menu uu wo _ W ho mm
13. The 3 TFT Display shows the current status information and is used with the Keyboard to adjust instrument settings and fully operate the instru ment in stand alone mode without a PC required The Front Cover has a view panel so that the important parts Pumphead and Purge Valve are always visible to the operator In case of a leak it can be detected before solvents are leaking out of the bottom of the Front Cover The Front Cover can be opened to easily access the Pumphead Purge Valve and capillary connections Element 5 9425 HPLC PUMP SYSTEM 13 Removing the Front Cover The Front Cover of the 5 9425 HPLC Pump System is completely remov able at its hinges Open The Front Cover to 90 in order to get free of any instrument stacked on top e Remove the Front Cover Store the Front Cover at a safe place 14 3 1 2 Back Panel Description The back panel of the 5 9425 HPLC Pump System houses the power and interface connectors and several drain outlets The Power Cord Connection amp Power Switch housing holds the main fuse in an internal fuse carrier The optional Drain Outlet is the leakage drain for the Gradient Mixer Module The optional Gas Outlet is the gas outlet of the Vacuum Pump where all solvent fumes from the degassing process are exhausted The digital I O and other interface connectors are used for remote instru ment control and are discussed in a later chapter
14. can be freely adjusted An optional integrated vacuum degasser removes dissolved gases in the mobile phase and prevents air bubbles in the system 2 1 1 Pump Mechanic The pump mechanic is a robust design for long lifetime and minimal Stepper Motor The is driven by a high power stepper motor The stepper motor Lubrication in nce gas has a much better resolution the The camshaft is constantly lubri low flow range than a conventional cated within a sealed chamber to Stepper Motor DC motor guarantee long lifetime and low maintenance The stepper motor driven camshaft driving the pis tons is optimized for the typical analytical flow range especially in the lower flow rate regions Optional Active Piston Backflushing The pump head incorporates an au tomatic piston backflushing system this system is interchangeable with old pumps and does not require an additional motor Permanent Lubrication The camshaft and piston drive is permanently lubricat ed within a sealed chamber The special lubrication used makes the Dual Piston Pumphead pump suitable for 24 7 operation 111211 pumphead for low pulsation Active Piston Backflushing Together with electronic pressure compensation the pumps are The optional piston backflushing actively flushed the piston after the pri suitable for all analytical tasks in mary seals to prevent crystallization of buffer
15. ct the Program Number 1 8 which should be run Prog Edit Select the Program Number 1 8 to edit see below Enter Gradient In this menu the Gradient Program can be edited The Program Number is selected in the Menu above Editing Values Each value of a Gradient Program line can be edited with the EDIT key and the UP and DOWN keys Confirm the change with EDIT and cancel the change with CENCEL key Adding Lines A new line can be added by pressing the EDIT key when the cursor is in the first column Deleting Lines A line can be deleted by pressing the CANCEL key when the cursor is in the first column 33 34 5 3 5 Submenu Degaser Settings Degaser Select lt ON gt or lt OFF gt to switch the degaser on or off Mode Select the degasser mode HYSTERESIS mode switches the dgeasser on and off depending on the vacuum level In CONTINUOUS mode the vac uum pump runs constantly Speed The speed of the vacuum can be selected to be either HIGH or LOW This speed setting has no impact on the degassing performance just on the time needed to reach the vacuum level Vacuum Level The current vacuum level is displayed 950 vacuum chamber pressure 5 3 6 Submenu Systemmenu Int Ext Ser The Operation Mode can be changed here between Intern Extern or Serial Software Display The Software Display is the installed firmware version of the Display PCB
16. direction HH o 0 OQ 45 Element 1 PEEK sealing ring E 1 Valve bearing with ring 5 marker Sapphire seat BM Ruby ball 3 5 Check guide made of ceramic 46 APPENDIX A COMPRESSIBI A general problem for constant flow delivery with piston pumps is the compressibility of the solvents under pressure Any liquid shows a specific volume elasticity If the liquid is influenced by pressure changes Ap the volume will change by AV The volume V will become the same as before if the pressure will be reduced to the original value again The dimension of the change in volume is the compressibility This can be shown as relative change of the volume ibility Ro cce necessary pressure change therefore X V Ap The constant volume delivery can be seen as a stepwise displacing of liq uid out of the pump head The dimension for the volume delivery is the amount of piston volume during a period of time But this is only correct as long as the delivery is done without any added pressure As soon as the liquid delivery has to be done against a back pressure a specific amount of the piston volume has to be used for compressing the liquid first before the actual delivery can start This can be described by the following diagram I D C 7 suction of liquid during pressure pl compressing the liquid from p1 to p2 delivery against pressure p2 changin
17. ected to the Vacuum Chambers 5 and the gas outlet on the back panel The Vacuum Chambers 5 are mounted on a drain tray and are connected to the vacuum pump and the Controller PCB The Mixing Chamber 6 is mounted on a drain tray and connected to Sol vent Inlet Block on the front panel and the Vacuum Chambers 5 The Pump Mechanic 7 drives the pumphead and includes the camshaft lubrication chamber driving pistons and the stepper motor Element Vacuum Chambers 4 6 Mining Chamber 19 20 4 INSTRUMENT SETUP 4 1 Unpacking Remove the S 9425 HPLC Pump System from its package and put it on the working desk Check the instrument thoroughly for any damage that may have occurred during shipping Contact your supplier in case of any damages Check the accessories shipped with the instrument if everything is com plete and in good condition 21 4 2 Capillary Connections 4 2 1 Isocratic Version The next step is to make all fluid connections The following list describes all necessary steps to make the proper capillary connections e Connect the 1 8 PVDF tubing to the Pumphead inlet 2 Fix the 1 8 capillaries with the Capillary Holder 1 Connect a 1 16 capillary Micro Analytical I D 0 5mm Semi Preparatibe I D 0 75mm to the Purge Valve Outlet 5 this capil lary is connected to the autosampler or manual injection valve Element
18. f this manual is subject to change without notice This docu ment is believed to be complete and accurate at the time of publication The Manufacturer is not liable for any damage resulted from the use of this manual 1 1 1 Symbols Throughout this manual important text sections are marked with the fol lowing symbols This section includes important information for the proper opera tion of the instrument Failure to follow this information may result in faulty behaviour of the instrument and or wrong analysis results This section emphasis some detailed information intended to optimize the performance of the instrument or to give a better understanding of some technical details 1 2 Safety Information This instrument is compliant with all related standards as stated in Ap pendix B 1 2 1 General Safety Information The operation of any analytical instrumentation requires the operator to be familiar with the potential hazards of using chemical solvents To avoid personal injury and or damage to the instrument the operator is responsible to follow all safety information herein The manufacturer assumes no liability for any damage resulted from not following any of these safety procedures 1 2 2 Intended Purpose This instrument is designed and certified as a general purpose laboratory instrument for research and routine analysis work only It is not certified for in vitro or other medical applications Any use outs
19. g from delivery to suction Element suction volume suction pressure delivery volume delivery pressure 47 48 The compressibility will effect the constant of the liquid delivery depending on the pressure To overcome this problem the 5 1125 is using a calcula tion program to correct the pressure depending change of the flow rate This calculation program corrects the compressibility as well as the always existing leakage rate of the check valves in relation to the actual pressure The processor is checking the back pressure every 0 1 seconds and corrects the piston speed accordingly The calculation program is using the liquid with the smallest compressibil ity water as a factor of 1 As different organic solvents are showing a different compressibility the processor needs this information for the most accurate delivery rate This information can be added through the Compressibility Factor in the menu As water has been normalized to the factor of 1 all others have to be small er than 1 The following table shows the Compressibility Factors of the mostly used solvents Solvent Compressibility For solvent mixtures of different organic solvents the constant can be cal culated by adding the constants of the different solvents in relation to their percentage in the mixture For example 50 H20 20 Methanol 30 Acetonitril 0 5 F H2O 0 2 Methanol 0 3 Acetonitril F 0 5x 1 0 0 2 x 0
20. ide this intended purpose does not fall with the manufactur 8 liability 1 2 3 Environmental Safety Only operate the instrument in well ventilated areas If volatile or flam mable solvents are used with this instrument arrange for proper disposal of any waste and or fumes Always properly dispose any waste solvents Avoid open flames and sparks when working with flammable and volatile solvents In case of instrument leakage turn off the instrument and remedy the leak age problem immediately 1 2 4 Electrical Safety Always use the provided power cords Replace faulty power cords and other cables before operating the instru ment Always replace blown fuses with original spare fuses When the instrument s housing is open electrical connections will be ex posed Disconnect the instrument from the main power before opening the housing The housing should only be opened by certified service personnel Damage of the instrument of injury may result from improper han dling 2 INSTRUMENT OVERVIEW 2 1 General Instrument Overview The 5 9425 HPLC Pump System is a very flexible and powerful HPLC 01 vent delivery system The system is available as Isocratic HPLC pump and Quaternary Low Pressure Gradient Pump with optional integrated online vacuum degasser The Quaternary Low Pressure Gradient version incorporates an active low pressure mixer with adjustable mixing volume The mixing chamber volume
21. ng party The doc ument is subject to periodical checks and can never reach an unchangeable state Version Release Date Description 0 9 2012 07 30 Preliminary Release 1 0 2012 10 25 First Release 53
22. posed of and not evaporated into the working area e Connect the supplied silica tubing to the DRAIN outlet on the back side of the instrument In case of a leakage of the Gradient Mixer or Vacuum Degasser solvent will be leaking through this tubing Make sure that the liquids are collected in some vessel and properly disposed of Element o MAINS e 50 60 Hz POWER 100 240 V FUSE 2 0AT GAS e OUT m E 1 S N a 950 s8r SA TET SY 3110W33 24 4 3 2 Electrical Connections The Drain and Gas Outlets are only connected in the Quaternary Gradient version Connect the supplied power cord to the Mains connector 1 Connect the supplied RS 232 cable to the RS 232 connector 3 if the instrument is to be operated by PC e Connect the remote control wires to the Digital I O connector 2 if the instrument is to be run in External mode Please refer to 5 Instrument Operation for further information about PC control and Remote control 5 50 60 Hz POWER 100 240 V FUSE 2 0 AT 5 m o x a S Pd z d amp 1 e o0 GAS 9 S N E el L Element 5 USB Communication not in use 25 26 4 3 3 Remote Connector Run Input Used to start the pump with the current settings EXTERN contact see below must be closed to activate this feature Extern Input The EXTE
23. remains in the rinsing chamber The rinsing of the chamber should be done with the plastic syringe deliv ered with the instrument 7 1 3 Change of Piston Ring Loosen the two hollow screws 10 for removing the mounting plate 9 take off the guide bearing piston assembly pressure springs and centering discs e pull out the piston guide pull out the piston rings very carefully with the help of a pair of tweezers completely insert the new sealing rings into the opening flange up ward the small spring has to show in direction of the pump head insert the piston guide upward with the secondary sealing ring white put the ceramic piston into the guide bearing insert the spring with the centering discs in the piston and place the whole unit on the piston guide put the mounting plate on top and fasten it with the hollow screws 10 e completely push down both pistons by hand for several times in order to check if the pistons were jammed during the process of as sembling 7 1 4 Replacing Check Valves The check valves are constructed as cylindrical cartridges The cartridges have sealing rings made of PEEK mounted on both sides 44 These sealing rings have to ensure that the solvent will not bypass the check valve Both valves on the high and low pressure side of the pump are iden tical and therefore can be used for both sides Place the cartridge in the valve housing and fasten fir
24. rnary Gradient Module is incorporates an active mixer with assembled on a stainless steel tray adjustable volume for optimized with a separate drain to protect the gradient mixing instrument in case of leakages 11 material The inner diameter and wall strength of the Teflon AF capillary used in these chambers is optimized for best efficiency with low volume Teflon AF is as chemical compatible as normal Teflon but has a much higher gas diffusion rate making a capillary 1000 times more efficient Vacuum Degasser Working Principle The solvent flows through a short length of Teflon AF capillary inside a sealed chamber This chamber vacuum chamber is completely sealed to the environment and vacuum is applied with a pump This vacuum pump decreases the pressure inside the chamber to near vacuum Due to this vacuum any dissolved gases in the solvent running through the inner capillary are removed through its semi permeable membrane wall The high efficiency of the Teflon AF material allows the usage of a very short length of capillary inside the vacuum chamber This low dead volume offers a quick solvent exchange and very short equilibration time Vacuum Sensor Vacuum Pump 12 3 INSTRUMENT DESCRIPTION 3 1 General Instrument Description 3 1 1 Front Panel Description The front panel of the 5 9425 HPLC Pump System consists of three main elements the TFT Display 1 the Keyboard 2 and the Front Cover 3
25. solutions The piston back HPLC and GPC 10 flushing is incoporporated into the pumphead and does not require any additional pump or motor Because of this all pumps are upgradable to active piston backflushing at any time without downtime Pumphead The short stroke dual piston pumphead is optimized for low pulsation and accurate delivery The 5 9425 HPLC Pump System can be fitted with any of the following pumpheads e Analytical Pumphead max Flow Rate 10 000 ml min e Micro Pumphead max Flow Rate 4 000 ml min Semi Preparative Pumphead max Flow Rate 40 000 ml min In addition to the performance types above all pumpheads can be deliv ered in e Stainless Steel e PEEK Titanium on request The different pumpheads should not be exchanged freely on a specific pump as the flow rate is adjusted to a specific type of pumphead When the pumphead is changed without proper flow adjustment the flow rate will not be accurate 2 1 2 Quaternary Gradient Module The S 9425 HPLC Pump System with the Quaternary Gradient option in cludes a Quaternary Gradient Module The whole module is mounted in side the pump and consists of several elements Active Gradient Mixer The active mixer has a variable volume mixing chamber with a magnetic stirrer unit built in The mixing volume can be adjusted freely to optimise mixing performance for different kind of solvents and applications The solenoid valves of the
26. ssure threshold is met the pump stops if the pres sure stays below the threshold for 30 seconds 41 42 7 INSTRUMENT MAINTENANC 7 1 Pumphead 7 1 1 Pumphead Assembly The following diagram shows all the components of the dismantled pump head Element Element Outlet valve housing pressure Piston guide with piston back side flushing Capillary tube for connecting the damping piston 4 Secondary sealing ring Hollow screws M4x45 Ceramic piston assembly Relief valve block 7 Guide bearing Centering disk Sealing ring relief valve Capillary for connecting relief valve and pump head Drain capillary from relief valve block 11 Check valve cartridge 12 Inlet valve housing suction mm 1 1 6 A 7 4 5 8 9 0 s I 20 EJ 1 1 2 22 8146 23 4 13 Ferrule 1 8 2 43 7 1 2 Piston Backflushing When using saliferous eluents a growth of salt crystals is possible behind the piston ring on the ceramic piston Under unfavorable working condi tions these salt crystals can lead to a higher wearing of the piston ring Generally it is sufficient to rinse the rinsing chamber between piston ring and secondary sealing ring with distilled water once a week The water remaining in the rinsing chamber stops the crystallization of salt crystals Therefore the lower capillary tubes should be connected together with PTFE tubing so that the water
27. st by hand and then turn another half of a turn by using the 13mm wrench delivered with the instrument If the pump is not delivering the correct flow rate the valve housing might not be tightened enough Before tighter fasting make sure that the pump was carefully flushed Cleaning the Check Valve Cartridge Generally the check valves cartridges don t wear However a deposit of dirt in the valve can influence the function In this case only a limited improve ment will be achieved when cleaning the fully assembled cartridge The more dependable method is to dismantle the valve for cleaning In order to avoid any loss of valve parts it is recommended to use a small container for the process is dismantling e pull out both sealing discs 1 carefully push out the valve contents 3 5 clean the valve part depending on the degree of dirt either with a washing bottle or with an ultrasonic bath insert the sealing disc which is next to the ring marker then insert the sapphire seat with the polished side toward the ruby ball place the ruby ball in the deeper side of the check guide 5 and put both into the bearing 2 with the ruby ball 4 facing the sapphire seat 3 press the second sealing disc on top After assembling check the functioning of the valve by blowing air through it It is possible to blow the air from this side of the ring marker through the valve and it should lock when blowing the other
28. ump with maximum flow rate and can damage the column if the Purge Valve is closed 5 2 Status Screen 28 The Status Screen shows the most important parameters Mode Intern Status STOP Mode Intern Status RUN Mode The top line shows the currently selected mode Intern Extern or Serial Status On the top right the current status is displayed Stop Hold Run or Error Flow The Flow Rate is shown on the left center area It always shows the current Flow Rate Pressure The current pressure is shown in the right center area The pressure is shown in the selected unit e g Bar MPa or PSI 5 3 Menu Description With the MENU key the Main Menu is displayed Use the CURSOR key UP and DOWN to browse through the Main Menu for access of one of the Submenus 29 30 5 3 1 Submenu Pump Menu gt Pump Settings Min Pressure The Minimum Pressure threshold The pump will stop if the pressure falls below this threshold Max Pressure The Maximum Pressure threshold The pump will stop immediately if the pressure rises above this threshold Max Pr Purge The Maximum Purge Pressure threshold The pump will stop immediately if the pressure rises above this threshold when the Purge function is used This a safety feature to prevent column damage when the purge valve is closed while Purge is active Change Unit The Pressure Unit can be changed here Available selections are
29. y suck the eluent through the tubing till it starts filling the syringe keep the syringe on the purge valve outlet e press PURGE and check if the syringe is filling with constant speed Now the pump is primed and ready for operation 38 6 3 Operating the Pump in Isocratic Mode 6 3 1 Starting the Pump The 5 9425 HPLC Pump System can be started by pressing the START key The pump will run at the selected flow rate Flow Start Ramp If a time is set for the Start Ramp the flow rate will slowly increase from 0 to the selected flow rate over a selected time e g Start Ramp time This feature gently increases flow and therefore pressure and may increase the lifetime of some specific columns 6 3 2 Stopping the Pump The 5 9425 HPLC Pump System can be stopped by pressing the STOP key The pump will stop immediately unless a Stop Ramp is set Flow Stop Ramp If a time is set for the Stop Ramp the flow rate will slowly decrease from the selected flow rate to 0 over a selected time e g Stop Ramp time Maximum Pressure In case the Maximum Pressure threshold is met the pump stops immedi ately Minimum Pressure In case the Minimum Pressure threshold is met the pump stops if the pres sure stays below the threshold for 30 seconds 39 6 4 Operating the Pump in Gradient Mode 40 Mode Intern Status STOP 6 4 1 Starting the Pump The S 9425 HPLC Pump System can be started by pressing
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