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333 and 334 Pumps User's Guide

1. ASCII characters is returned n l Reset Audit Trail configuration parameters index Response format n if log file exist N if log file does not exists N l Read Audit Trail configuration parameters Response format nnn mmmm where nnn identifies the parameter see E command mmmam is the value This command is similar to the immediate E command but returns information from the configuration recorded in the log file at the starting time Only the designated parameters L type are available If the pump data base is busy the response is In this case send the command again later Comment Use the immediate n command first to set the index to the first parameter in the table The index is set to the next available parameters after each reading In case of error the response is 0 B Set Audit Trail files index Syntax On where n sets the stored file index ranging from 0 to 9 At the starting file time the running file and its linked files 10 files maximum are stored with the log file This command sets the file index used by the O immediate command and resets the Audit Trail file event index used in the o immediate command O l Read Audit Trail files Response n m p q where n File number ranging from 1 to 24 any other value means the file does not exist m 0 if file is not locked m 1 if it is locked p Nb of loop q Linked file 255 if there is no linked fi
2. Command Type Description N E SSECH AWNOOVCOCOZSKRA CO LTIDQODATAAMMIIAAy ves XX WW W D DW DW DWO W W W WD WW oD Request module identification Define Module identification Master reset Pump status Application control Reset maintenance counters Read maintenance counters Dims or brightens front panel display 833 Pump only Read file directory Assigns a value to a parameter Read the value of a parameter Set pumping parameters Returns pumping parameters Write application event into Edit file Read application event from Edit file Reset Application event index Delete application event from Edit file Write contact inputs 833 Pump only Read contact inputs 333 Pump only Read contact input buffer 333 Pump only Write contact outputs 333 Pump only Read contact outputs 333 Pump only Read contact output buffers 333 Pump only Input remote keystrokes Read key entry Reset Audit trail configuration parameters index 333 Pump only Read Audit trail configuration parameters 333 Pump only Set Audit trail files index 333 Pump only Read audit trail files 333 Pump only Read audit trail files events 833 Pump only Enter pressure value Read pressure value Buffer status Read Audit trail line 333 Pump only Reset audit trail file line index 833 Pump only Delete Audit trail file 333 Pump only Write display 333 Pump only Read display 833 Pump only
3. 3 Extended capabilities for solvent selection are offered by the addition of a Solvent Valve Block SVB to any of the configured pumps A1 to A4 B1 to B4 C1 to C4 Figure opposite shows how the addition of a Solvent Valve Block SVB could be used to test the effectiveness of different solvents selected successively The solvents are routed via suitable tubing to the SVB which performs all of the required switching functions at low pressure no mixing takes place between solvents connected to a valve block Three typical configurations are described in the following Sections 1 Binary Gradient or an isocratic mixture of two solvents 333 334 Pumping System or ternary gradient 333 334 334 Pumping System 2 Injection Configuration 333 334 Pumping System and 30X injection pump 3 Binary Gradient controlled from a PC 333 334 Pumping System Connecting Tubing GORM Installation Ai E TMU E au SHUI Mt nt Configuration Example 1 Binary Gradient or Isocratic A 333 Pump may be set up to control the flow and composition on a time variant gradient or a time invariant isocratic basis when associated with a 334 Pump Thus you can pump gradients using two solvents or you can pump in isocratic mode after mixing A from one pump B from the other For a binary gradient configuration install a 333 Pump Master at the left and a 334 Pump Slave at the right although the slave pump could be a
4. 4 21 Software Entering Method Programs 4 22 1 Press Pump Edit you see the Pump Control screen Screen 2 you may be presented with the following soft keys at one time or another File to access file operations Edit Create to review or modify a Method Program or View to review a file that can t be modified Create Edit to begin editing a Method Program Config to enter a configuration parameters for the currently selected Edit File GLP to access audit maintenance run in and test functions for a 333 Pump Watch to obtain post run information 2 With the cursor on Edit file key in the number of the file that you wish to edit or create For a new file the number is contained by square brackets 3 Press Create or Edit for an existing file you see the Edit Method screen Screen 30 the possible soft keys are Events to access or enter a list of events Link to link the file currently selected to another file No Link to undo a link with another file Consump to see the predicted fluid consumption for the file currently selected Creating and Editing Method Programs Entering Events With reference to the following figures starting at Screen 30 press Events or Select you see the Edit Method File screen Screen 39 you will be presented with soft keys for the following event types FLOW to schedule the flow rates COMP to schedule a change in the
5. Tubing downstream from the filter 2 1 x 3 2 mm 1 8 Nut 316 steel 1 4 28 TPI for 3 2 mm 1 8 tubing Ferrule 316 steel for 3 2 mm 1 8 tubing Total Pressurized Volume 10 4 ml inside 333 Pump 17 ml inside 333 334 Pumping System Additional Components Solvent Selection Valve Block Identification Gilson E66465 plus serial number Reference includes holder four inlet tubings and filters tubing and Tee piece for connecting to pump heads Flow path materials PTFE Number of ports one outlet and four inlets to select one solvent out of four Internal volume 240 yl total per channel including 80 pl in common path 3 2 mm diameter through holes On line Vacuum Solvent Degasser Identification Gilson 864 Degasser Gilson E66250 plus serial number Flow path materials PTFE and PPS Number of channels four Internal volume 9 2 ml per channel Pressure drop lt 25 hPa for water at 10 ml min Vacuum 69 72 hPa Maximum flow rate per channel 50 ml min for water and 10 ml min for organic solvents to maintain the flow rate accuracy of 333 and 334 pumps Residual concentration of dissolved oxygen oxygen saturated water 1 ml min 25 C lt 0 4 ppm for a single channel lt 0 2 ppm for two channels in series Power consumption 32 W Size 80 width x 150 height x 260 depth mm Weight 3 kg Reference Information Wear Parts Outlet filter piston seals inlet check valves
6. Mbar Mbar Mbar 0 to 2000 see notes 0 to 2000 see notes 0 to 2000 see notes 0 to 2000 see notes 0 to 2000 see notes 0 to 2000 see notes 0 to 2000 see notes 0 to 2000 see notes 0 to 2000 see notes 0 to 2000 see notes 0 to 2000 see notes N sduind ree pue ggg 10 spuewwog GSIOC Commands for 333 and 334 Pumps Command Type Description Code Type Parameter Units Range 91 R W L Pump C selector C4 Solvent Compressibility K Mbar 0 to 2000 see notes used only if solvent selector is fitted to Pump C 96 R W L Injection pump liquid compressibility K Mbar 0 to 2000 see notes 100 R W L Pump A selector A1 Solvent Name See Table amp notes 101 R W L Pump A selector A2 Solvent Name See Table amp notes 102 R W L Pump A selector A3 Solvent Name See Table amp notes 103 R W L Pump A selector A4 Solvent Name See Table amp notes 104 R W L Pump B selector B1 Solvent Name See Table amp notes 105 R W L Pump B selector B2 Solvent Name See Table amp notes 106 R W L Pump B selector B3 Solvent Name See Table amp notes 107 R W L Pump B selector B4 Solvent Name See Table amp notes 108 R W L Pump C selector C1 Solvent Name See Table amp notes 109 R W L Pump C selector C2 Solvent Name See Table amp notes 110 R W L Pump C selector C3 Solvent Name See Table amp notes 111 R W L Pump C selector C4 Solvent Name S
7. Multiples Submultiples Factor Prefix Symbol Factor Prefix Symbol 10 deka da 10 deci d 10 hecto h 10 centi c 10 kilo k 10 milli m 10 mega M 10 micro u 10 giga G 10 nano n 10 tera T 10 pico p 108 peta P 1075 femto f 10 exa E 1078 atto a 107 zetta Z 107 zepto Z 10 yotta Y 104 yocto y suyun pue SUOI USAUOD jeuoneoN Overview Introduction Overview User s Guide Description and Applicability This user s guide is both for 333 Pumps and for 334 Pumps Information that applies uniquely to one or other of these models is clearly identified at the appropriate point Except for the absence of two components no distinction is made at the hydraulic level between the 334 extra solvent remote controlled pump and the 333 primary solvent master pump so much of this type of information e g Chapters 2 and 5 relates to both 333 and 334 Pumps There are differences at the physical and electrical level 334 Pumps have no control panel or output connector so the information relating to the pump s software e g Chapter 4 is only directly relevant to a 333 Pump Chapter 1 contains brief descriptions of 333 and 334 Pumps together with unpacking instructions and warranty details Chapter 2 contains descriptions of 333 and 334 Pump s major components Chapter 3 contains instructions for installing and setting up 333 and 334 Pumps Ch
8. Running a Method Program 4 42 Pump file 19 000 ml min 0 0 A 0 0 B Screen 1 Screen 2 File 19 post run information Minimum pressure 0 Maximum pressure 6 Piston cycle time 0 01 bar 9 bar A 0 01 B Information Transfer Gilson software is supplied with each 333 Pump to transfer information between a 333 Pump and a computer This diskette based Pump Data Transfer PDT software is for use on a Personal Computer PC or similar running under Windows 95 or higher Data transferred from the pump may be printed out from the PC or saved as files In addition previously saved Configuration and Method Files may be transferred from a PC to a pump Connections 1 Using a Gilson 605 Adapter For simpler systems or where control is normally from the 333 Pump s keyboard a 605 Adapter is normally sufficient Your computer must have at least one serial communications socket When connecting a Model 605 to an IBM PC or equivalent having a 9 pin RS 232 output a 9 pin D female to 25 pin D male converter is required i Connect the 9 pin female end of the converter to the 9 pin male RS 232 socket on the PC ii Connect the 25 pin female end of the Model 605 to the 25 pin male connector on the converter iii Connect the 9 pin female connector of the Model 605 to the 9 pin male GSIOC socket on the right hand 9 pin male GSIOC socket From Controller on the Master 333 Pump iv Whe
9. 3 Configure the Master 333 Pump 4 Prime the hydraulics initialize and run in the piston seals if new Starting and Stopping a Run Switch on the Model 333 Pump then after initialization you see the ready to run screen Screen 1 Before starting the run you may see the following soft keys Pump Edit to access pump operations Detect to access an associated detector Manual to prime and operate manually Run to run the current Method Program file Zero to zero the detector signal if associated 1 The cursor indicates the currently selected file number to select a different file key in its number then press ENTER 2 Press Run you will see the following soft keys at one time or another Edit to view or modify any file during a run it may be another file Pause interrupt the Method Program pumping continues Resume to continue a paused Method Program End to stop the Method Program file pumping continues Stop to stop pumping the Method Program may continue A weiboig poyan e Buluuny 4 39 Software Running a Method Program 4 40 4 After pressing Run the ready to run screen dynami cally displays the flow rate and composition of the mobile phase and displays the pressure detected by the pressure sensor The top line of the screen is reserved for information from a 15X detector if connected If you press Pause the Method Program is interrupted but pumping continues at the
10. A locked file is indicated by an asterisk before the file number Pressing either key returns you to Screen 11 Copy To copy a file press Copy Screen 14 key in the number to which the currently selected file will be copied A message appears asking you to confirm your actions normally press Yes Or if in the destination file already exists press No unless you want to over write the existing file Care overwritten files cannot be recovered Pressing either key returns you to Screen 11 Links To see how the existing files are linked press Links the following screen Screen 12 shows the order in which the linked files will be run Chain circular means that you have cross linked files resulting in more than one occurrence of one or more file numbers in the series Take care when linking files Bad links can lead to unforeseen consequences Linking to a file that does not yet exist is not allowed You should consider carefully your linking strategy create and check the files before linking them see Linking Files Software Good Laboratory Practice GLP Functions All of the following functions are available where control is from a 333 Pump UniPoint users should refer to the UniPoint User s Guide for Audit Trail and Maintenance related functions a Audit trail records the sequence of events that take place during a run when you execute one or more Method Program files Audit trails are
11. SD lt 1 or 0 1 MPa whichever is greater Residual pulsation amplitude according to the volume of liquid pressurized downstream from the pump recorded from pin 10 lt 0 1 MPa for 200 ml 40 x 250 mm column lt 1 or 0 3 MPa whichever is greater for 10 ml 20 x 50 mm column lt 9 or 1 3 MPa for 50 pl 0 25 x 1000 mm tubing Flow Rate Selectable units liter h and ml min default ml min three significant digits Adjustment increment 0 01 ml min Adjustable range from 0 02 ml min for one solvent up to 599 ml min for three solvents at 33 3 each Single Solvent 333 Nominal range 0 2 200 ml min Accuracy bias lt 1 or 5 3 pl min whichever is greater Repeatability SD lt 0 5 or 2 7 pl min whichever is greater lt 0 2 specified for 5 50 ml min after a run of gt 30 minutes with a new piston seal Two Solvents Mixed Under Pressure 333 334 Nominal range 2 200 ml min up to 400 ml min for 50 B Accuracy bias lt 2 or 53 pl min whichever is greater mass flow rate at constant temperature Repeatability SD lt 0 7 or 27 pl min whichever is greater Composition and Mixing Number of solvents three A B and C each one selectable out of four using the solvent selection valve block supplied as an additional accessory for each pump Reference Information Composition increment 0 1 Dwell volume total system volume from mixing point to filter outlet 2
12. a is the pump head identification B for the 2 pump heads working in dual piston mode b is the mode F for flow mode cccccc is the flow value in tenth of l min Range 333 334 0 to 2000000 331 332 0 to 500000 for each pump If cecccc 0 the pump head s stop s and goes to its rest position ppp is the working pressure in tenth of MPa In HPM mode with a solvent valve block installed the software opens the valve port where the percentage is not equal to 0 and closes the other 3 ports If dddd eeee ffff 0 valve port 1 is opened If dddd is not equal to zero valve port 2 is opened If eeee is not equal to zero valve port 3 is opened If ffff is not equal to zero valve port 4 is opened Other pumping parameters such as head size liquid compressibility and inlet pressure for the dual piston mode must be defined using the buffered E command before to use the F command Note the time interval between two buffered F commands must be at least 0 01 min Returns pumping parameters Response format abc where a is the piston mode D for Dual piston mode b is the right head status F if the 2 heads dual piston mode are running in flow mode S if the 2 heads dual piston mode are stopped E if one of the two head motors is jammed dual piston mode Add application event in Edit file Syntax G type time p1 p2 p3 where type is the event code time is the event time in hundre
13. dismantling maintenance adjustment and repair should only be performed by personnel trained in such work and who are aware of the possible dangers involved Neither a 333 Pump nor a 334 Pump nor the pump heads may be sterilized using an autoclave or any other device When you Symbol Explanation need to clean a pump use one of the three following methods Alternating current iadan dry doth PROTECTIVE CONDUCTOR 2 a cloth dampened with water TERMINAL 3 a cloth dampened with soapy water E If a cloth dampened with soapy water is used to Off Supply switch clean the pump only domestic soap may be used No other form of detergent or chemical may be used Caution risk of electric shock These electronic and hazard symbols appear on the pump ie es a Caution refer to User s Guide Safety 2 Declaration of Conformity Application of Council Directives 89 336 EEC and 73 23 EEC Standards to which Conformity is Declared Electromagnetic Compatibility EN 50081 1 1992 and EN 50081 2 1992 for emission EN 50082 1 1998 and EN 50082 2 1995 for immunity Safety EN61010 1 1993 including AMD A2 1995 UL 3101 1 1993 and CAN CSA 1010 1 1992 including MOD2 1997 Manufacturer Gilson S A 72 rue Gambetta BP45 95400 Villiers le Bel France Type of Equipment Laboratory Equipment Product 333 and 334 Pumps Beginning with Serial Number 196534 for 333 and 196540 for 334 I the u
14. for 333 and 334 Pumps 866149 Bottle tray 33X Pumps 410706 Inlet filter 316 steel 20 um 5 16 24 TPI 4 8 mm tubing no fitting 420606 Tubing FEP 3 2 x 4 8 mm 3 16 per meter H3 inlet 410450 Nut POM white 5 16 24 TPI 4 8 mm 3 16 tubing Upchurch P138 410451 Ferrule ETFE natural 4 8 mm 3 16 tubing Upchurch P133N 410108 Plug PVDF natural 1 4 28 TPI 410472 Plug POM white 5 16 24 TPI Upchurch P557 410449 Plug POM white 5 16 24 TPI with 1 mm through hole E66381 Inlet tubing FEP 3 2 x 4 8 x 1250 mm H3 pump head includes 1 x 410706 Inlet filter 316 steel 20 um 1 x 420606 Tubing FEP 3 2 x 4 8 x 1200 mm 3 16 H3 inlet 2 x 410450 Nut POM white 5 16 24 TPI 4 8 mm 3 16 tubing Upchurch P138 2 x 410451 Ferrule ETFE natural 4 8 mm 3 16 tubing Upchurch P133N E66379 Plumbing kit piston rinsing chambers 333 and 334 Pumps includes 1 x E66316 Tubing FEP 2 x 3 x 830 mm 1 8 right 1 x E66317 Tubing FEP 2 x 3 x 930 mm 1 8 left 2 x E66389 Tubing FEP 3 2 x 4 8 x 234 mm 3 16 preshaped 2 x 410429 Ferrule ETFE natural 3 2 mm 1 8 tubing Upchurch P300N 2 x 866183 Drain nut PCTFE natural 5 16 24 TPI 4 8 mm 3 16 tubing with seal E66183 Drain nut PCTFE natural 5 16 24 TPI 4 8 mm 3 16 tubing with seal 866067 Bellows fluoroelastomer piston rinsing chamber H1 H2 H3 pump heads 866160 Drip pan PP w
15. representative The solvent valve block replaces the plate that can be seen just above the drip tray Pump Head Installation The pump heads are pre installed However for routine servicing you will need to remove the pump heads refer to Chapter 5 Accessories Installation 3 12 Accessories Additional accessories may be obtained from Gilson these are a degasser a column holder a holder for a manual injection valve and a shelf to enable you to stack 333 334 Pumps and 15X Detectors This shelf is designed to support the weight of the pump and solvent bottles Assembly consists of using the supplied screws to attach four legs to the metallic tray Space is available between the legs for a detector or a 30X Pump The solvent bottle tray which is supplied as a standard accessory is easily fitted to both 333 and 334 Pumps Degasser Please refer to the User s Guide of the Gilson 864 degasser Column Holder The column holder attaches to the left side of the pump Three pairs of column support fitted with clips for different diameter columns are provided in the kit Column Support Retaining Knob Knurled Screw Installation Holder Installation 1 Loosely fit the retaining stud 2 Slide the studs into the tops of the retaining slots at the side of the pump 3 When the holder is correctly positioned fully tighten the retaining knobs Support Installation 1 Push one of a pair of colu
16. 10 the test is successful For a successful test OK is displayed on the screen otherwise FAILED is displayed Check for leaks before repeating the test Starting from the GLP Screen 82 press Leak Screen 260 you will see these soft keys at one time or another Start to start the test pump starts End to end the test pump stops 1 The outlet from the pump filter should be sealed with plug supplied before running the test 2 Maintain or modify the proposed values for flow rate 0 5 ml min and pressure 15 MPa 3 Press Start to start the pump or End to stop the pump in an emergency 4 Press ESC to return to Screen 82 Mixing Test This test is based on an ASTM method for determining the linearity accuracy and repeatability of a binary composition gradient The test automatically implements a program consisting of three loops Starting from the GLP Screen 82 press Mix Screen 270 to perform the binary mixing test For details refer to the document entitled Operational Qualification Procedure reference 804041 Software Running a Method Program Preparing for a Run In addition to creating your Method Program file the following steps must be completed before running a Method Program 1 Make the electrical and hydraulic connections between the pump s and other equipment in the system as described in Chapter 3 2 Connect the power and switch on all of equipment
17. 333 and 334 Pump User s Guide The instruments described in this document are piston pumps which should only be used in an indoor environment for pumping purposes by qualified personnel If a 333 Pump or a 334 Pump is used in a manner not specified by Gilson the protection provided by the pump may be impaired Voltages present inside the 333 and 334 Pumps are potentially dangerous If there is a problem with any pump the power cable should be removed until qualified service personnel have repaired it This is to prevent anyone from inadvertently using the pump thus causing possible harm to themselves or damage to the pump itself The leakage current of a 333 Pump and of a 334 Pump is within the limits allowed by safety standards of laboratory equipment An efficient ground connection is imperative for the physical protection of the user Power supply cord reference 500005 is for use in France and Germany Power supply cord reference 500006 is for use in USA and Canada For other countries contact your local Gilson distributor The maximum voltage for any electrical device connected to each input or output contact of a 333 Pump is 48 V However adequate protection including clothing and ventilation must be provided if dangerous liquids are used In case of incidental spillage carefully wipe with a dry cloth taking into account the nature of the spilled liquid and the necessary safety precautions Safety 1 Safety Cleaning
18. Chapter 6 contains comprehensive lists of items supplied as standard and additional accessories plus a list of recommended spare parts Installation 3 Your 333 or 334 Pump is delivered with its principal hydraulic components already installed You are advised to read this section which contains important information relating to both 333 and 334 Pumps instructions are given for installing accessories where appropriate The software described in this Chapter is for users for whom a 333 Pump is the controlling device If your controlling device is a PC using for example Gilson s UniPoint Software you should refer to the documentation relating to UniPoint The key steps the minimum necessary to configure the pump s from a Master 333 Pump are given in this Chapter for full details of 333 software refer to Chapter 4 Here is a summary of the key steps 1 Electrically connect the 333 or 334 Pump and any associated components a detector other pumps etc connect them to a suitable power supply and switch on all components 2 If control is from a Master 333 Pump check or enter the configuration details using the control panel on the 333 Pump If control is from PC based software e g UniPoint refer to the user s guide for the controlling software 3 Make the hydraulic connections to the 333 and 334 Pumps and their associated components then prime the pump s refer to Chapter 4 You are then ready to enter or activ
19. File numbers 21 to 24 are reserved for safety files therefore they should not be assigned to Method Programs You should create Safety Programs for files 21 24 in the same way that you create Method Programs In each case if you do not create the file an error message will be displayed on the screen and the pump will stop If file 21 is being executed the pressure limit is automatically raised by 10 then if the new pressure limit is passed the pump stops juod Hunni Software Configuring When the low pressure limit is crossed by decreasing values the effect is delayed by 0 3 of a minute whatever be the effect stop pumping if file 22 is empty or start file 22 if you have defined it The delay is to allow the Method Program to continue if a fugitive air bubble creates a brief and abrupt pressure decrease Changing the Pressure Limits The maximum values for these limits are configuration dependent High limit gt Low limit 1 Key in the new value for High 0 to 21 MPa starts file 21 press ENTER 2 Key in the new value for Low 0 to 60 MPa starts file 22 press ENTER 3 Press Next to configure the Other safety functions Other Safety Functions One function is predetermined you cannot change Input 2 close starts file 24 After a power failure you may choose to stop the pump continue with the file Method Program that was running at the time of the failure or start
20. Program currently running The pause may be configured Chapter 4 with or without flow With flow means that pumping continues at the rate and composition that existed at the time the pause was initiated when resume is signaled the Method Program continues from the same point INPUT WAIT Input 1 An external relay contact connected to this input may be used to signal to the Method Program currently running the 333 Pump that the external equipment e g fraction collector sampling injector is ready EMERGENCY Input 2 Closing an external relay contact connected to this input may be used to signal to the pump software to start a Safety Program file file 24 oO SUOIJEDIUNWIWOD SUOI DOUUOD e2913 3 5 Installation Electrical Connections Communications 3 6 GSIOC Connections When connecting more than two pieces of equipment by GSIOC cable the devices should be connected linearly i e in series using shielded Y type Gilson cables reference 500933 This type of cable has a pair of female and male 9 pin D connectors at one end and a second female connector at the other You will need one less cable than the number of devices being connected The first pair of devices in the chain are connected using the female sockets at either end of the cable Then for the third and subsequent devices you connect another cable between the male socket on the GSIOC cable and the appropriate socket on t
21. Stop then undo both purge line connectors Water will run from each purge line into the drip tray the rinsing lines and rinsing chambers will fill with water When you see bubble free water in the rinsing lines and that air is no longer exiting from the head via the purge lines close both purge lines In use water from the small bottle rinses the piston although it is a closed circuit you may need to change the water from time to time and of course repeat this procedure Injector Connection Connect the appropriate tubing to the outlet filter of the 333 Pump OO Installation Drip Tray The removable drip tray fitted to the pump is supplied as standard The drip tray slots into the well at the bottom of the pump Installation consists of lifting up the tray fitting one end with a length of tubing The other end of the tubing goes to the drain or a suitable receptacle via the drain tubing exit port Installation is completed by replacing the drip tray SUO I D9UUOD JIjNepAH Solvent Valve Block Installation A solvent valve block is available as an optional extra it may be used to test the effectiveness of different solvents or to perform rinsing cleaning and conditioning The liquids are routed via suitable tubing to the valve block which performs all of the required switching functions at low pressure under software control Exit Port Drain Tubing This item would be pre installed by your Gilson
22. and disconnect it from the power supply 3 Remove the back panel to which the fan is attached by undoing the retaining screws The mounting screws for both heads are now visible 4 Insert a 3 mm Allen wrench into the mounting screw turning it in the clockwise direction until you reach a stop you will hear a thump as you hit the stop At this point the piston engaging mechanism will be withdrawn to a maximum distance into the interior of the pump motor Then turn the wrench two turns counterclockwise Maintenance and Troubleshooting 5 Disconnect all solvent lines from the pump head s in question 6 Progressively remove each of the two screws securing the pump head to the pump motor using the supplied 5 mm Allen wrench Support the pump head with your other hand after loosening the two screws moderate force is required Disassembling a Pump Head The following steps should be carried out on a clean dry surface No special tools are required 1 Undo the two retaining screws using a3 mm Allen wrench as supplied 2 Remove the white cap and retaining screws 3 Pull the piston and bellows out of the body of the pump head 4 Pull apart the two halves of the pump head with a slight twisting motion 5 Inspect the bellows for damage if this component needs to be replaced use your thumbs to push it firmly away from the retaining collar When remounting the pump head you can leave the mechanism a
23. another Change to select the pump head then press ENTER to confirm Solvent A Pump 1L 1R Solvent B Pump 2L 2R Solvent C Pump 3L 3R Dismount to move the pump head pistons to the dismount position End to finish the dismount procedure Logs to review and reset the pump head logs Software Dismount Procedure Caution The dismount procedure should only be carried out by suitably qualified people The pistons must go to the dismount position before you can physically remove the head s from the pump 1 After selecting a pump head press Dismount then press ENTER 2 You now see Screen 250 before pressing Yes check that it is safe to set the piston in motion 3 Wait while the piston moves to the dismount position Screen 254 until you see the message Change heads Screen 252 4 Remove the pump head carry out the required servicing see Chapter 5 Maintenance and refit the pump head 5 When done press End wait while the pistons move into position Screen 254a until you see the message dismount heads Screen 256 6 If you have finished press No to return to Screen 84 and ESC to return to Screen 82 Maintenance Logs You use this function to view the log of wear parts for any configured 333 or 334 Pump The log contains the usage of the part to date hours the user set upper limit hours or the number of operational piston cycles that the part has completed megacycle one
24. chromato graphic results by removing dissolved gasses from solvents down to less than 0 4 ppm for oxygen dissolved in water at a flow rate of 1 ml minute It is compatible with 33X Pumps up to 10 ml min 50 ml min with water to maintain flow rate accuracy NO s u uodwo jeuondo 2 5 Description 333 Pump Control Components 2 6 333 Pump Control Components The components for controlling from a 333 Pump are at the front of the instrument All electrical connections are made at the rear Control Panel Display Unit Screen Keypad Display Unit and Screens The 40 character 8 line unit is used to display sets of information parameters commands messages time related events flow rates solvent composition in run information etc and soft key functions A screen comprises of a set of information depending on the software and the choices that you make Each screen has a unique number accessible by pressing the HELP key Keypad and Function Keys Soft keys The bottom line of the display unit is reserved for labeling six variable function soft keys identified by the six evenly spaced circles just below the display unit The functions of the soft keys which are determined by the software may change from screen to screen For any given screen the current function is displayed above each active soft key Inactive keys have no function displayed Description Pressing a soft key selects
25. cmt crecesnncn cr 5 2 Normal Dismounting Procedure ssssssssrottrttrstessreseeseess 5 2 Alternative Dismounting Procedures a heretics 5 2 Disassembling a Pump Heads ees e corer cacatc es 5 3 Replaciny aiPiston seal man 5 4 Piston Rinsing Chanabet 22002050000000000000000709020000072000000000000090000000 5 4 Riston anc Below sa ccnc cs cee E ete 5 5 Reassembling a Pump Head sce e cece neces 5 6 Check Valves asc ee eee eee eee eects 5 8 Cernig a Check Valve arr cc cs s css ssayeaeseasesesessestucscraestaetteces 5 8 Table of Contents 3 Replacing a Check Valve ma 5 9 Ae A A EE 5 10 Inlet ikilters meee e a cee 5 10 Outlet Eter a eraser ean A A 5 10 Troubleshooting soera ness aay cesses ens sioseaitaeeearas 5 11 Brrr LED S33 UMM d 20000002000000200000500100000000090000000000000000000000 5 11 ErronNlessagesi Ooo BUMP nearer see eters 5 12 Electrical amp Program Problems 2 cncccaace cee 5 13 Ty eiratilie PEODIGIS cananaa cencuaveecimsatismencas os 5 14 6 Reference Information Technical Waitara sce senses ace esses eect eeee senses 6 2 Gilson 333 and 334 33X Pumps cssscssectscesccsrssessessetsessasese 6 2 Working Range amp Performance Data eie sstear ss 6 3 Coritwol Characteristics 7004 baie atcieaniycuomoruret 6 6 Hydraulic Components a 6 9 Olay RESTOR CES co ceasasesnssesesescesrvsscoessssecsnssesesesasannstises ses 6 11 Environmental Conditions nee es 6 12 olen MiseIDilitye aeaea OEE 6 13 Blow Rate
26. e g Ryton from Phillips Petroleum Polytetrafluoroethylene e g Teflon from Du Pont de Nemours UHMWPE Ultra high molecular weight polyethylene oe sjeayeyy jeonsejdouuey 10 Suoieinaiqqy Part Numbers Reference Information 6 20 Part Numbers Pump Standard Accessories and Documents are supplied as standard Additional Accessories Wear Parts and Replacement Parts are available from your Gilson distributor Gilson 333 Pump Reference Description E66013 333 Pump 110 and 220 V single solvent 200 ml min 21 MPa Gilson 333 Pumps can accept any electrical voltage from 90 to 260 V 50 or 60 Hz Each is supplied with two power cords part number 500006 for 110 V and 500005 for 220 V Standard accessories Reference Description Quantity Hydraulic 866149 Bottle tray for 333 and 334 Pumps 1 EF66381 Inlet tubing FEP 3 2 x 4 8 x 1250 mm 3 16 with filter for connecting to pump tee piece 1 E66391 Tubing 316 steel 2 1 x 3 2 x 500 mm 1 8 1 73 ml to injector 1 430057 Tubing 316 steel 1 x 1 6 x 600 mm 1 16 471 ul to injector 1 E66394 Tubing 316 steel 0 13 x 1 6 x 185 mm 1 16 2 ul pre shaped GLP Seal 1 E66384 Adapter 316 steel 1 4 28 TPI male amp 10 32 TPI female 1 mm through 11 ul 1 E66379 Plumbing kit for piston rinsing chambers connect to pump heads 1 E66386 Bottle glass 180 ml pierced PE cap screwed cap for piston rinsing solvent 1 410
27. flammable solvants the following table gives safety data according to the following definitions and references Definitions 1 The flash point FP is the lowest temperature at which a substance or mixture in an open vessel gives off enough combustible vapors to produce a momentary flash of fire when a small flame is passed near its surface 1 2 A substance is classified as flammable if its FP is lower than 38 2 3 The auto ignition temperature AIT is the lowest temperature at which a substance can self ignite at atmospheric pressure without an external ignition source The determination of AIT is rather imprecise and apparatus dependent Nevertheless the AIT indicates the maximum allowable surface temperature of equipment and apparatus when exposed to air vapor mixtures of these substances 2 4 An explosive atmosphere consists of a mixture of the vapor of a flammable substance being at a temperature higher than its FP with air at a concentration within the limits of flammability LOF 3 Volatile does not imply flammable for example dichloromethane is volatile but is non flammable _ 2 2 amp a 2 si e e es e se ele Seales ee ese Miers TE Ee Lu lt 2 ae ar Lu Q BP C 78 65 82 66 822 69 98 77 35 VP hPa 93 169 118 216 60 202 55 121 735 FP C 12 11 6 14 12 22 4 4 45 AIT C 490 510 520 320 54
28. gradient and maintains during 10 minutes the flow rate at the value that generated this pressure otherwise it goes to the flow rate indicated in the table and maintains it during 10 minutes At the end of this time the flow rate linearly decreases to zero in 2 minutes Implementation The flow rate and pressure values see table below used by the pre stored procedures are implemented through two soft keys GLP Seal and GLP Leak Flow Rates and Pressure Values F and P Implemented by Pre stored Procedures GLP Seal and GLP Leak Refer to Implementation above Prime GLP Seal GLP Leak Pump Head F Purge F Procedure F Procedure P Procedure P Procedure F Fixed Fixed Default Default Default Default ml min ml min ml min MPa MPa ml min 33X H3 50 50 15 15 15 0 5 33X H2 35 35 25 45 45 0 5 30X 5 5 3 75 5 45 45 30X 10 10 7 5 10 45 45 30X 25 25 18 75 12 21 28 30X 50 50 22 5 12 10 5 14 30X 100 100 22 5 12 5 2 7 30X 200 200 22 5 12 2 6 3 5 A Software GLP Seal uses the supplied capillary 0 13 x 1 6 x 185 mm ref E66394 which is to be connected at the outlet filter and water as the recommended solvent In these conditions the pressure is generally reached before the default flow rate GLP Leak uses the supplied plug ref 410478 which must be connected at the outlet filter You can select any configured pump The parameters are adjusted automatically by the software Starti
29. is for use in France and Germany Power supply cord reference 500006 is for use in USA and Canada For other countries your local Gilson distributor can advise you concerning the type of power connector to use Input Output Signal Connectors 333 Pump The two sockets use the 14 pin and 10 pin connectors supplied with your 333 Pump GSIOC Connectors The 9 pin socket s accept standard GSIOC connectors The 333 Pump has two connectors To Slave and From Controller the 334 Pump has one connector From Controller and two switches for setting GSIOC parameters SW UNIT ID SETTING SW BAUD RATE Swi Swi ct HTG Bao o EXTERHAL s Only use standard GSIOC Gilson Serial Input Output Channel connectors GSI0C FROM CONTROLLER age k a a N s u uodwos 01 U0D dwnd gge Accessories Description 2 10 Accessories The standard accessories supplied with the pump include plumbing items tools and electrical connectors Additional accessories to be ordered separately include solvent valve block solvent degasser an injection valve holder extra plumbing items a column holder electrical interfaces and cable kits A shelf is available on which the pump can be placed allowing a 30X Pump to be placed underneath A diskette is supplied containing Gilson s Pump Data Transfer Software which enables the user to download information from a 333 Pump to a Personal Computer PC
30. on a 334 Pump is labelled Remote on a 333 Pump it is labelled Error Installation Electrical Connections Communications You need to connect GSIOC cables between the pumps make connections to the detector and make any single wire contact connections for input output signals which may be necessary for communicating with other equipment Contact Connections Input amp Output The input and output contact functions are shared between two terminal blocks 14 pin and 10 pin situated on the pump s back panel The maximum input voltage for any electrical device connected to each input or output contact is 48 V Legend NO Normally Open GROUND Common NC Normally Closed COM Common z D oS gt N E 0 Volt From Controller START END PAUSE RESUME EMERGENCY ances a 5 a GSIOC 5 N Se pr B 2 2 ae 5 5 5 5 Ej 5 5 5 5 3 8 es 8 393 2 BR 8 oO O oO oO a 14 pin Connector 10pin Connector In order to connect signal wires to the terminal blocks you must first fit the appropriate connector as supplied in the standard accessories package The 14 pin connector fits the left hand socket and the 10 pin connector fits the right hand socket After gently pushing each connectors into its socket you can connect wires to the appropriate terminal To connect a wire to the terminal you should strip back the wire s protective cove
31. parameter code from 100 to 111 overwrites the corresponding values for both K and X Solvent and Mixture Codes for Parameter Codes 100 to 111 116 Solvent Code Other 0 Water 1 Methanol 2 Acetonitrile 3 Tetrahydrofuran 4 lsopropanol 5 Hexane 6 Dichloromethane 7 Mixture Code Mixture Code Water acetonitrile 10 90 20 Water methanol 10 90 30 Water acetonitrile 20 80 21 Water methanol 20 80 31 Water acetonitrile 30 70 22 Water methanol 30 70 32 Water acetonitrile 40 60 23 Water methanol 40 60 33 Water acetonitrile 50 50 24 Water methanol 50 50 34 Water acetonitrile 60 40 25 Water methanol 60 40 35 Water acetonitrile 70 30 26 Water methanol 70 30 36 Water acetonitrile 80 20 27 Water methanol 80 20 37 Water acetonitrile 90 10 28 Water methanol 90 10 38 E l Read value of parameter Response format nnn mmmm where nnn identifies the parameter see above mmmm is the value If the pump data base is busy the response is In this case send the command again later Comment Use the buffered Ennn command first to specify the parameter to be reviewed To read an application first send the editing file number and then read all parameters see also read application events command N sduind peg pue ggg 10 spuewwog GSIOC Commands for 333 and 334 Pumps 7 18 Command Type Description F Set pumping parameters Syntax Fabcccccc ppp dddd eeee ffff Where
32. press ENTER to confirm If no SVB is fitted you can skip this step in which case you see only one solvent channel per pump A B or C for each of which you may select the solvent type and enter a value for Inlet Pressure 3 For each solvent channel A or A1 to A4 B or B1 to B4 C or C1 to C4 use the arrow keys to select a solvent name or enter a value for compressibility press Change to select another solvent press ENTER to confirm For more see Named Solvents Compressibility below and for full details refer to Chapter 6 4 Optionally for each single solvent channel pump you may key in a value for Inlet Pressure 0 50 MPa that is the pressure at the inlet to the pump Merion tani pump NO head This option is not offered when you have Controlled pump 33X Maximum number of solvents TWO configured an SVB Safety 1 0 Misc Change Hard Hyd Screen 50 Configuration Screen 90 Screen 91 Solvent A Head type H3 Solvent valve block NONE ER Solvent B Screen 60 Adjust hydraulics Initialize piston before injection NO Software Adjusting the Hydraulics Press Adjust to access Adjust Hydraulics screen Screen 60 in order to access the following Initialize piston before injection only if Injection from pump YES Initializing the piston of the injection pump 30X can improve injection precision at low flow rates set to YES Configuring an Inject
33. pressure 0 60 MPa Manual Control Operations prime flow rate and electrical output contacts Prime carried out at 50 ml min successive or simultaneous for each channel oe Reference Information Operating Programs Application methods mobile phase flow rate and composition constant or multi segment linear gradient sample injection from extra pump digital coordination with detector signal autozero and lamp switching coordination by electrical contacts with other instruments programmable solvent selection with additional valve block safety maintenance and mixing test see below 20 files of 30 steps with indication of solvent consumption eed jed1UYyoeL Mixing test pre stored binary gradient profile according to the ASTM E 19 09 07 2 for the evaluation of the range of composition linearity and of the composition accuracy and repeatability using 20 steps and selectable flow rate Safety methods four files of 30 steps pressure limits emergency and power failure anomaly processing procedures with related outcomes including red light indicator beeper alarm pumping stop end of program display of specific message defining the anomaly and edition of this message in an audit trail which can be printed out from a PC Pump Data Transfer software supplied 605 interface required Watch function post run information displaying minimum and maximum pressures plus piston cycle times for iso
34. recoverable by the PC based Pump Data Transfer software supplied with each 333 Pump From the Control Panel of a 333 Pump you can only activate or deactivate the audit trail function and adjust the date and time b You can access the pump s maintenance logs for the Master 333 Pump and its Slave 33X Pump if connected via GSIOC and activate the dismount function When replacing any 333 or 334 Pump head you are obliged to use the dismount function in order to be able to physically remove the head from the front of the pump c New piston seals should be run in after installation The seal installation procedure prepares the piston seals in advance of a full run in 10 to 12 ml min using methanol or isopropanol d Leak is used to check the watertightness of the hydraulic circuit e A pre programmed qualification test is available to test the mixing functions of the Master 333 Pump Procedure Switch on the 333 Pump then after initialization you see the ready to run screen Screen 1 1 Edit Pump to access pump operations you see the Pump Control screen Screen 2 2 Press GLP you see the GLP screen Screen 82 the possible soft keys are Audit to access the audit trail functions Maint to verify maintenance logs or dismount a pump head Seal to install the piston seals Leak to test the hydraulic circuit Qualif to perform the qualification test A suonoun 99119814 10 e10qe po
35. safety file 23 To select the required option 1 With the cursor at When power restored after failure starts file 23 press Change 2 At the required option STOP CONTINUE SAME FILE START FILE 23 press ENTER 3 With the cursor at Malfunction sounds beeper alarm press Change 4 At the required option YES NO press ENTER 5 Press ESC to return to Screen 50 Caution File numbers 21 to 24 are reserved for the safety features described here However these files do not exist until you create the Safety Programs You must ensure that any Safety Programs that you create and save as files 21 to 24 function correctly and provide the desired level of protection A Software Electrical Contacts Press I O you see the Electrical Contacts screen Screen 70 which allows you to modify certain options related to electrical signals see Electrical Connections Communication Buun uo Screen 50 Poono Seen Model 333 Model 333 H3 nee mp YES Injection on pump YES Controlled pumps 33X H3 33X H3 3 Controlled pumps Bax H3 33X H3 30X 10 Maximum number of e THRE Maximum number of solvents THREE Safety 1 0 Misc Change Hard Hyd Safety 1 0 Misc Change Hard Hyd Screen 70 Electrical contacts Input pause WITH FLOW Contact pulse duration 1 00 min Analog output signal A a You may either continue with or stop the flow when an input pause signal is received b You may set the len
36. the function displayed directly above it for example Edit Create and Run Descriptions of these and all other soft key labels are given in Chapter 4 Fixed function keys In addition to the variable function soft keys there are fixed function keys as follows HELP to display advice at any time with no effect on the operation of the pump ESC to change from a software level to a higher one or quit a HELP screen CLEAR to cancel your last entry before it is stored in the memory ENTER to confirm a selection or value and store it in the memory Arrow keys 4 to move from one variable field to another screen dependent Numeric keys 0 to 9 and to enter values for predefined parameters Stand by Panel The stand by panel comprises an ON OFF key and three Light Emitting Diodes LEDs iar 1 The POWER LED green lights up when the main ON OFF switch is set to ON eligi Sm on 2 The ON LED yellow lights up when the main EE ERROR ON OFF I O switch is set to ON I and the k ON OFF key on the standby panel is set to ON pressing the key toggles between ON and OFF 3 The ERROR LED red lights up under certain anomaly conditions see Chapter 5 The ON OFF key on the panel is for use when you want to turn off the power for a short period of time or to stop the 333 or 334 Pump instantaneously When you want to turn off the power for a longer period of time you sho
37. the outlet tubings Inlet tubing is loose Nut and or ferrule damaged Tighten the connectors Replace the nut and or ferrule Inlet filter is plugged Clean or replace the inlet filter s Refill time is too short Increase the refill time see Chapter 4 Config Hyd Air bubbles in the outlet tubing only Loose connection of outlet Tighten connectors Leaks from a pump head Defective piston seal Replace the defective seal Abnormally low flow rate Leaks Check the hydraulic circuit for leaks Air entering upstream from the head Check the upstream connections Plugged inlet filter Replace inlet filter Defective check valve Replace check valve Incorrectly mounted pump head Remount the pump head Abnormally high pressure Plugged outlet filter Clean or replace outlet filter Column particle size too small or plugged column Replace check valve Change or flush column Mobile phase viscosity too high Use lower viscosity solvents or increase temperature Baseline noise periodic pulses see Chapter 4 piston cycle time Mixer volume too small Increase mixer volume Air in the hydraulics Prime the pump degas the solvent Faulty pressure module Contact your Gilson representative Reference Information This Chapter contains Technical Data Lists of Parts and after Referen
38. then press ENTER 3 For a new event after Add press Confirm to affirm the values entered 4 Press ESC to go back to Screen 30 sweibojg poya Huaug COMP 1 Key in a time 0 00 to 9999 minutes then press ENTER 2 Key in a percentage 0 to 100 for solvent channel B then press ENTER 3 Key in a percentage 0 to 100 for solvent channel C if configured 4 For a new event after Add press Confirm to affirm the values entered 5 Press ESC to go back to Screen 30 WAIT 1 Key in a time 0 00 to 9999 minutes then press ENTER 2 Press Change to select either CLOSE or OPEN 3 Press Confirm to affirm the value entered or CLEAR to abort the value 4 Press ESC to go back to Screen 30 OUTPUT 1 Key in a time 0 00 to 9999 minutes then press ENTER 2 Key in an output contact number 1 to 4 then press ENTER 3 Press Change to select either CLOSE OPEN or PULSE see Section 4 2 2 for pulse length 4 For a new event after Add press Confirm to affirm the values entered 5 Press ESC to go back to Screen 30 4 25 Software Entering Method Programs 4 26 Depends on the injection volume entered previously INJ You enter one injection event per loop specifying the time at which the injection starts and the volume to be injected The third parameter can be either the required flow rate or the length of the injection duration If you enter the require
39. 0 260 230 490 190 LOF 3 19 7 36 3 16 212 212 18 1 7 2 11 2 36 e2 S UBAJOS jqewwueL 4 10 eed 3JeS Reference Information Safety Data for Flammable Solvents References 1 H Bennett Concise Chemical and Technical Dictionary Edward Arnold Ed 1986 2 W E Baker et al Explosion Hazards and Evaluation Elsevier Sci Publ 1983 3 Union des Industries Chimiques L Electricit Statique en Atmosph re Explosive Septembre 1982 4 D R Lide Handbook of Chemistry and Physics 79 ed CRC Press 1998 1999 5 G W C Kaye and T H Laby Tables of Physical and Chemical Constants 16 ed Longman Ed 1995 6 B P Mullins Spontaneous Ignition of Liquid Fuels Butterworths Ed 1955 7 Chemical Safety Sheets Working Safely with Hazardous Chemicals Kluwer Acad Publ Samson Chem Publ Dutch Inst for the Working Environment and Dutch Chem Ind Assoc 1991 8 F A Williams Combustion Theory Benjamin Cummings Publ 1985 Reference Information Abbreviations for Thermoplastic Materials EP Ethylenepropylene ETFE Ethylenetetrafluoroethylene FEP PCTFE PE PEEK POM PP PPS PTFE e g Tefzel from Du Pont de Ne mours Fluoride ethylenepropylene Polychlorotrifluoroethylene e g Kel F from 3M Polyethylene Polyetheretherketone Polyoxymethylene e g Delrin from Du Pont de Nemours Polypropylene Polyphenylene sulfide
40. 1 At Screens 35 or 36 use the vertical arrow keys to scroll through the list of events 2 With the cursor at the line corresponding to the event that you want to delete press Delete 3 At Screen 37 press Yes to confirm the deletion returns to Screen 35 or No to return to Screen 36 4 Repeat for other events if required and press List to review the revised Method Program file 5 When done press ESC to return to Screen 30 Software A Method Program Work Sheet m gt gt 7 gt File Number Method Name tas D SETUP PARAMETERS gt Oo Pressure High limit Low limit Q U Number of pumps Loops Link file Ps Pump Line Model Solvent D Refill Comp Head Size S A 3 B Cc D or Inj I O OPERATIONS Time Contact State Function PROGRAM STEPS Step No Time Event Operation Step No Time Event Operation 14 15 16 17 18 19 20 o NIJA AJOJN o are Oo M i wo 30 4 29 Software File Management 4 30 Pump file 19 000 mi min 0 0 A 0 0 B Screen 1 Screen 2 File Management The file management facility enables you to see a list of currently assigned files to copy lock delete and edit files Procedure Switch on the 333 Pump then after initial
41. 1 M of solute being solid in normal ambient conditions you must rinse the piston s when pumping using the same liquid but without the solute Maintenance and Troubleshooting To facilitate the required connections refer to Chapter 3 for the rinsing liquid a plumbing kit is available as a standard accessory ref E66379 You should change the rinsing liquid at least once a week Piston and Bellows Although the size and material of the piston shaft vary between different head sizes the procedure is the same to inspect and if necessary replace the bellows follow the steps shown in the figure a b c Use your thumbs to remove the bellows moderate force is required When removing the bellows support the piston by the head not by the shaft This advice applies mainly to the smaller and more fragile shafts such as those used to demonstrate this procedure in the figure H1 head the ceramic shafts of H3 heads are thicker and less susceptible to damage a H3 Piston Assembly b Removing the Bellows Mounting The Bellows 1 Insert the tool ref E66231 which ensures that the orifice at the end of the bellows remains open into the open end of the bellows d 2 Place the tool on a firm flat surface 3 Push down on the metallic ring using four digits e until the orifice grips the end of the tool on its own Refitting The Bellows 1 The tool which keeps the end of the bellows open enables the b
42. 333 Pump s Hydraulic Components Pressure Purge Mixng SM Purge Line The principal hydraulic components of a 333 Pump are pump heads PPMM and the outlet filter Construction characteristics are given in Chapter 6 Two reciprocating pump motors are contained within the body of the pump The tops of the pump motors protrude through the front panel For Pump 1 the filtered solvent line connects to the inlet tee outlets from the tee connect to the pump heads 1L and 1R thus the motors pump the same solvent A to the pressure module For Pumps 2 and 3 the heads are respectively designated 2L and 2R for solvent B plus 3L and 3R for solvent C Inlet Tee Pump Head L Pump Head R Pressure Purge and Mixing Module PPMM Three functions are combined in the PPMM a pressure transducer 0 60 MPa a static mixer to blend up to 3 solvents under high pressure 2 85 ml chamber volume a purge valve to manually switch the mobile phase between outlet filter and drain To operate the purge valve turn the black knob fully clockwise to direct the flow to the outlet filter fully counterclockwise to direct the flow to the atmospheric purge outlet Outlet Filter The outlet filter Upchurch A332 characteristics are 10 pm threshold 1 6 mm thickness 19 mm diameter and 160 pl total internal volume NO s usu0dWOD dIjneipAH S duindg EEE Description xe I o Solvent Outlet Line gt ai So
43. 333 and 334 Pumps User s Guide 4 GILSON SOLUTIONS AT WORK Fi YOU 333 and 334 Pumps User s Guide 801422B 2000 Gilson S A All rights reserved February 2000 Table of Contents Safety Declaration of Conformity 1 Introduction Notational Conventions and Units 1 2 Software Related Conventions 331 Pump sseseeeen 1 2 Units and Conversion Factors cesses ee 1 2 Oyerview e eaa 1 4 User s Guide Description and Applicability 1 4 HarcdwareiMescrip tOn Meer tienen cade re 1 5 331 Pump Software Description ncccareccs ects e 1 5 Opera tine Principle Pena 1 6 Unpacking oee e e E 1 7 Hardware neee cetacean nee arena eet 1 7 SOLU Walkers ieee dee seers eins cantare ate rea ase eon ecronie 1 7 Warranty a2 sacs cs viedeseesg sees E cacs bes EE E aS 1 8 Customer Service m ee a E ste 1 9 2 Description 331 Pump s Hydraulic Components soe scscesesesesscercces 2 3 332 Pump s Hydraulic Components cn e nese escuccs reise Pressure Node tics sit ien eae tees Astras eara 2 3 Outlet Filter 72 seers ea steer 2 3 Rump Heads meee e ecco asnvasssndsaneaased epasescsatessectanonsxs 2 4 Optional Cora NENS hisaas sores sees ts 2 5 DOIVENt Valve Block ee a nrda nica A 2 5 Solvent Degasser m r a oamer secur 255 333 Pump Control Components s usssssssssss11strsttrstrstrssrsssssnsssss 2 6 Croo EE eee ee ea ae aa 2 6 AEG E oa Panels E aneeae ee nee ugar 2 7 Rear Panel Electrical Connectors 2
44. 470 Nut 316 steel 28 TPI for 3 2 mm 1 8 tubing Upchurch C235 2 410471 Ferrule 316 steel for 3 2 mm 1 8 tubing Upchurch C236 2 410426 Nut 316 steel 10 32 TPI for 1 6 mm 1 16 tubing Upchurch U400 2 410425 Ferrule 316 steel 10 32 TPI for 1 6 mm 1 16 tubing Upchurch U401 2 E66463 OQ plumbing kit 1 Reference Information Reference Description Quantity Mechanical 610101 Spanner for tubing nuts 6 3 7 9 mm 4 5 16 1 610112 Spanner for check valve holder 14 mm 1 610117 Spanner for outlet filter double ended 11 and 13 mm 2 610043 Allen wrench 3 mm rear end to release pump head 1 610045 Allen wrench 5 mm front end to remove pump head 1 E66157 Tubing clip PP for 3 2 mm 1 8 for 333 and 334 Pump bottle tray 2 E66158 Tubing clip PP for 4 8 mm 3 16 for 333 and 334 Pump bottle tray 1 E66231 Bellows mounting tool POM white piston assembly for pump heads 1 Electrical 506341 Barrier strip connector 14 pin for output contacts 1 506367 Barrier strip connector 10 pin for input contacts and two outputs 1 500006 Power cord 110 V 1 500005 Power cord 220 V 1 Documents and Data Transfer Software Reference Description Quantity 804035 Quality control certificate 333 and 334 Pumps 1 None Quality control report 333 and 334 Pumps 1 801422 User s guide 333 and 334 Pumps 1 804040 Installation Qualification procedure 333 and 334 Pumps 1 804041 Operat
45. 8 Power CONRECIOE cscs O A OS 2 9 Input Output Signal Connectors 333 Pump s 2 9 GSIOC Connectors eect ne eee cree ees eerie ine 2 9 NTO T acer ens ete wie sete Ree eters eee 2 10 Table of Contents 1 3 Installation 4 Software Electrical Connections Switching On i recrc ccs crectss ess 3 2 Rower Supply e e cusmmecaaiiiates 3 2 Fuse Installation and Voltage Selection cssssserees 3 2 Switching ON eee e iniranarsten tacit 3 2 Electrical Connections COMMUNICATIONS cceeseeesees sees 3 3 Coritach ConmechOns e iavan nies cies sits eeninet 3 3 Powering an External Relay 2o sscssssssccecsseneesssesnsscrseereearssese 3 4 Oiio eaae E een meen 3 4 Inpat Signals e e E vey rr TS 3 4 GalO Conmect Ons ma have ae hts ence ovanwiess 3 6 GSIOC MID ee srecsscyesesesrnnaserssansoezasrnss a a 3 7 Dit Rate ee eet ie ees es ees ne re es 3 7 Twi TGP Systems nea ae ene eta Nec cae 3 8 Hy draulie GrmechiOns s gat sectcaer sna seisen ace uche 3 9 Solvent Inlet Lines e nsesertaaseeaceuptveccrssannssses 3 9 Piston Rinsing Chamber sine ce oar cers 3 10 Injector ConmechOnn cass cence aaneennny eae 3 10 Drip Tay oes occas e oncom acne oes erences EE 3 11 Solvent Valve Block linstallattonce gr ssecccetree sete ee 3 11 Pump Head Installston estes nie eas setae atas 3 11 PRE COSS IOS deee aeee a e e eee sere cerca cen mteeoe eee g 12 Degasser ee a A E EE 3 12 Column Holder ee eee 3 12 TIEA O E a Dae eE E A sess ar
46. 8 R W L Reserved for 32X 1 for solvent A 2 for solvent B 3 for solvent C 59 R W L Reserved for 32X 0 for automatic activation 1 for STOP 60 RL Type of pump A 2 DUAL 61 RL Type of pump B 0 NO PUMP 2 DUAL 62 RL Type of pump C 0 NO PUMP 2 DUAL 63 RL Reserved for 32X 0 NO PUMP 1 SINGLE 2 DUAL 3 P30X 64 RL Type of injection pump 0 NO PUMP 3 P30X 65 R W L Reserved for 32X 1 100 mi 0 to 9999 66 R W Keypad beeper 0 OFF 1 ON 67 R Control of pump channels 0 if controlled by see F Command the pump 1 if controlled via GSIOG 68 R Total flow of the pump 1 10 ul Same whether control see F Command is from pump or not 69 R Reserved for 32X 1 10 ul 71 RW L Flow unit 2 ml min 3 L h 72 RW L Volume unit O ul 1 ml 2 L 73 RW L Pressure unit 0 MPa 1 bar 2 psi GSIOC Command Type Description Code Type Parameter Units Range 75 RW L Pump A solvent selector 0 none 1 A1 2 A2 3 A3 4 A4 76 RW L Pump B solvent selector 0 none 1 B1 2 B2 3 B3 4 B4 77 RW L Pump C solvent selector 0 none 1 C1 2 C2 3 C3 4 C4 Parameter codes 40 41 and 43 refer to Edit application This application is defined by Edit Application number code 1 Comment if the value mmmmmm and the sign are omitted the value is unchanged but the command sets the parameter index to the specified parameter
47. Data Types Import Export Open Close Save Print Audit x xX x x X Method x x x x x x Config x X x x x x Counters x x Xx x x Drop down menus allow you to access the following data types Audit Trail Displays the Audit Trail File including the following tabulated headings Config Method and Log Config contains the information detailed below Main etc Method Displays graphical and numeric data of the transferred or opened method Config Displays parameters and data for the transferred or opened configuration The information is grouped under the following tabulated headings Main Safety Others I O Solvent A Solvent B etc Counters Displays the counters for the transferred or opened data set A weiboig poyan e Buluuny 4 43 Control of a Model 15X Detector Software 4 44 Control of a Model 15X Detector The following is a summary of information relating to Gilson Model 15X Detectors For complete information refer to the relevant detector user s guide Introduction Any one of the following Models can be controlled from a 333 Pump Model 151 Single Wavelength Detector with Control Panel Model 152 Single Wavelength Detector no Control Panel Model 155 Dual Wavelength Detector with Control Panel Model 156 Dual Wavelength Detector no Control Panel Control includes programming two events in the 333 Method Program detector signal
48. Head identification Counter code 0 for head A 0 for piston seal 1 for head B 1 for piston 2 for head C 2 for out check valve 4 for inj head 3 for in check valve J Counter limit as for event code i as for event code i kK Power failure 0 for STOP option 1 for Continue option 2 for start safety file T Audit Trail is full m Injection event n Loop file begin Loop number o Link to next file Link file A Pressure limit reached 0 for high pressure limit Pressure limit in safety file absent tenths of MPa 1 for low pressure limit Pressure limit in tenths of MPa B Power failure safety file absent Emergency input activated emergency file absent D Invalid conditions Flag reset by start a file or flow using the buffered F command E Hydraulic failed Pump Number 0 for pump A 1 for pump B 2 for pump C 4 for inj pump F Slave module absent Unit ID Running file does not exist H Validation process has restored parameters to the default values K Pressure limit reached 0 for high pressure limit Pressure limit in safety file already running tenths of MPa 1 for low pressure limit Pressure limit in tenths of MPa t l Reset Audit Trail line index Response format T if file exists N if file does not exists The Audit trail file is an event file Each line store one event This file is read via GSIOC event by event See immediate S command This command sets the index to the
49. L Pump C selector C2 Liquid Compressibility X Mbar 0 to 2000 see notes 140 R W L Pump C selector C3 Liquid Compressibility X Mbar 0 to 2000 see notes GSIOC Command Type Description Code Type Parameter Units Range 141 R W L Pump C selector C4 Liquid Compressibility X Mbar 0 to 2000 see notes 142 to 149 Reserved Notes 1 Concerning flow correction and pressure pulsation reduction if the solvent is one of the Named Solvents for parameter codes 100 to 111 116 the corresponding solvent code is sent see below When the pump receives the solvent code it sets coefficients K and X to their predefined values In case of an undefined solvent both the flow correction coefficient K Solvent Compressibility and the pressure pulsation correction coefficient X Liquid Compressibility must be sent to the pump 2 Writing aK value for any parameter code from 80 to 91 overwrites the current value and sets the corresponding Solvent Name to Other When writing K you must also send a value for X see parameter codes 130 to 141 3 Writing an X value for any parameter code from 130 to 141 overwrites the current value and sets the corresponding Solvent Name to Other When writing X you must also send a value for K see parameter codes 80 to 91 96 4 Except for Other writing a Solvent Name for any
50. Read display buffer 333 Pump only Read compression stroke N sduind peg pue ggg 10 spuewwog 7 9 GSIOC Commands for 333 and 334 Pumps 7 10 Maintenance Functions Command Type Description so7o aQa onaaqdnas5s mw WwWDndow WW Dismount Mount head Start maintenance sequence Calibrate pressure transducer Pressure transducer calibration status Leakage maintenance sequence status Run in maintenance sequence status This command is for Gilson use only This command is for Gilson use only This command is for Gilson use only Motor status Description of Commands Command Type Description Request module identification Response format xxx Va bc where Va bc is the software version and xxx is the pump identification string XXX 333 for 333 Master Pump XXX 334 for 334 Slave Pump Define module identification syntax is string where string 333 for 333 Master Pump string 334 for 334 Slave Pump Comment This command sets all parameters to the default value erases all applications erases all counter values Master reset returns and reset the machine in its power up state GSIOC Command Type Description Pump status returns abcde where a is the application status S for Stop R for Running P for Pause C for Conditioning only for maintena
51. This command increments automatically the application event index p1 to p3 are additional parameters depending of the event type The meaning and number of parameters depends on the event type Pump will return only parameters corresponding to event type Delete application event from Edit file Syntax Hn where nis the event index range from 0 to 29 Reset Application event index Response format H if there is at least one event N if there is no event or if application does not exists Application contains up to 30 events The application can be read back event by event This command sets the index to the first event if any Write contact inputs Syntax labcd where a is the input 1 Start End b is the input 2 Pause Resume c is the input 3 Wait d is the input 4 Emergency Parameters C for closed D for open X for state unchanged for reconnect to internal software Comment This command disconnects the input from the internal software if the corresponding parameter is C or D The value is stored in the contact input buffer s Read contact inputs Response format abcd as above for each input C if closed and connect to internal software c if closed and disconnect from internal software D if open and connect to internal software d if open and disconnect from internal software This command rea
52. XANE O0Cm0COC COCMa00C000n METHANOL Ongagcamqouaaao0lm MA METHYLETHYL KETONE J JO OOOOOOOOOOOOOO ocTANE CJ OOO SB OOOOOSBOOOOOOBOO Pame Cd J OOO OOOO BOOOOOO8OoOoO fsoPROPANOL J DOO OOOOOOOOOOOOOOOOOO DLPROPYLETHER TIO OOOOOOSSOOOOOOOOOOO0 TeTRAHYDROFURAN IO OOOOOOOOOOOOOOOOOOO0O0H MoWENE CJ OOOO OOOOOOOOOOOOOOOOoOoOoOo WaeR CN OOO OOOO SBREORBBORBOBO XE UJ ODO OOO OOOO BBOOOOOOOOOOOOOOsoO oll J u g Lu x i Fale S lt E olli JARRBERRBBBEBRRBREREEE AIE IE C misciBLE SEE eel eel ella eli mle ee Geek E immiscipe 6 13 Reference Information Flow Rate Accuracy Flow Rate Accuracy Principle 1 To generate the selected flow rate with the specified accuracy maintained under high pressure and for a variety of liquids the soft ware adds two complementary corrections to the basic piston flow rate Defined from the piston stroke volume only the piston flow rate is theoretically accurate only at atmospheric pressure The objective flow rate F is considered as the sum of three components F F F F F the piston flow rate decreases when pressure increases F the compensation flow rate for the liquid compressibility increases with pressure F the compensation flow rate for all other factors also increases with pressure The piston flow rate F is defined by F N V5 where N number of piston cycles per unit time and V 0 piston stroke volume 2 The compensat
53. a control panel integral keypad and screen for configuring programming and coordinating with other equipment pumps detectors injectors etc 334 Pumps are designed as slave pumps for delivery of a second solvent B and with two additional 334 Pumps a third solvent C to be mixed with the primary solvent A pumped by the 333 334 Pumps have no PPMM no outlet filter and because they have no control panel they are physically shorter They may be controlled by 333 Pump software using its control panel or by PC based software such as Gilson s UniPoint and GSIOC Gilson Serial Input Output Channel commands 333 Pump Software Description Although the pre installed software is designed to be user friendly you are advised to read this guide care fully before using the pump Programming consists of entering configuration details for your pump and then a sequence of events flow rate composition electrical contacts etc as a Method Program M lAJ9AQ Overview Introduction 1 6 By means of the pre installed software or PC based software a 333 Pump may be used to control a Gilson detector and up to three other pumps of the following types a 334 Pump Gilson 30X Series Pumps with any head or another 333 Pump If solvent injection is required the injection pump must be of the 30X Series Alternatively you may use Gilson UniPoint System software to control 333 and 334 Pumps and associated Gilson equipme
54. a key Otherwise 0 disables the screen saver Changing the Screen Contrast Press either of the horizontal arrow keys lt 4 gt until you arrive at a suitable level This is shown as follows Screen display contrast where the marks the current setting Changing the Units 1 Starting at Screen 75 press Units you see the Select Units screen Screen 80 2 With the cursor at Flow rate ml min press Change to select ul or ml then press ENTER 3 With the cursor at Pressure MPa press Change to select MPa or psi or bar then press ENTER 4 With the cursor at Injection volume press Change to select yl or ml or T then press ENTER You may also use the vertical arrow keys A and W to move the cursor from one parameter field to another but you must first confirm the previous selection by pressing ENTER 5 Press ESC once to return to Screen 75 twice to return to Screen 50 Beeper Status 1 Starting at Screen 75 press Other you see Screen 76 2 Use Change to set the keypad beeper to either ON or OFF 3 Confirm your selection by pressing ENTER 4 Press ESC to return to Screen 50 Software Manual Operations Manual Operations Introduction The following manual functions are available a Prime the channels must be done for a new pump or pump head b Pump solvents at a specific flow rate and composition t
55. ain module and accessories The original packing should be kept especially for the period during which the instrument is under warranty in case the equipment has to be returned to the factory Because of their weight about 35 kg 44 kg packed you should take special care when handling the large cartons Pump modules are heavy and should be lifted from the carton with care by two persons Instructions describing the unpacking procedures are to be found on and in the carton Software The software is pre installed and is accessible using the control panel immediately after switching on a 333 Pump Huryoedun Introduction Warranty Warranty If the pump does not appear to function correctly first verify the electrical connections are correct and that the instrument is switched on Contact your Gilson distributor for technical advice or possibly a service visit Any service required will be given within the warranty conditions assured by your Gilson distributor Introduction Customer Service Gilson and its worldwide network of authorized distributors provide customers with four types of assistance sales technical applications and service Customer Service personnel are able to serve you more efficiently if you provide the following information 1 The serial number and model number of the equipment involved 2 Type of computer if used available memory microprocessor and software version s in operatio
56. ainty in measurement attributable to the measuring procedure e Limits of acceptance for the results specified in the individual Quality Control Report supplied with each pump and in the Operational Qualification Procedure to be implemented by qualified personnel Gilson 333 and 334 33X Pumps Type of Pump Gilson 333 Pump is a primary solvent master pump equipped with a control panel and a pressure purge and mixing module PPMM Gilson 334 Pump is a secondary solvent remote controlled pump without a control panel and without a PPMM Both are single solvent dual piston reciprocating pumps 200 ml min and 21 MPa Each pump is factory fitted with two H3 pump heads Up to three 33X Pumps including one 333 Pump because it is fitted with a PPMM can be associated to deliver three solvents mixed at high pressure flowing up to 599 ml min at 33 3 of each Use of Pumps For preparative scale HPLC 33X Pumps may be used with 20 to 100 mm bore columns Le Reference Information For each configured pump a Solvent Valve Block SVB is available as an additional accessory a SVB enables four solvents to be switched under software control twelve solvents for three associated pumps For isocratic mobile phases one pump is used giving single solvent delivery under high pressure with flow rate and event programming including solvent switching if a SVB is fitted Beg jed1UYydEL For composition gradient mobile p
57. am injector solvent line A to the inlet tee piece on 333 Pump solvent line B to the inlet tee piece on 334 Pump special tubing ref E66360 from the outlet tee piece of the 334 Pump to the inlet of the 333 s PPMM prime the system dn bulyas 3 25 Installation 3 26 Software 4 1 Software Using the Control Panel 4 2 For the screens that illustrate this Chapter the soft key to press is indicated by the lighter color soft key follow the path indicated by the arrows When you should press other control panel keys e g ENTER these are indicated in bold at the appropriate point Using the Control Panel The control panel consists of a display unit and a keypad Display Unit The 40 character 8 line display unit is used to show time related events flow rate solvent composition in run information and so on The bottom line of the display unit is for labeling six variable function soft keys Keypad The soft keys are identified by the six evenly spaced circles just below the display unit Pressing a soft key selects the function displayed directly above it for example Edit Manual and Run Descriptions of these and all other soft key labels are given later in this Chapter Where a soft key may take an alternative label the alternative is shown in between parenthesis for example Edit Pump In addition to the variable function soft keys there are fixed function keys as fol
58. apter 4 contains details of the 333 Pump software used for configuration and control Directly this information only concerns 333 Pumps However there are implications for any 334 Pumps controlled from a 333 Pump If you use external software to control 33X Pumps up to three you should refer to the manual for the controlling software e g UniPoint Some supplementary information has been included relating to UniPoint and GLP functions Chapter 5 applies to 333 and 334 Pumps it describes preventive maintenance troubleshooting and procedures for dismounting the heads Introduction Chapter 6 contains reference information relevant to 333 and 334 Pumps specifications technical data hydraulic parameter information solvent miscibility and compressibility corrections and separate parts lists items and references for each pump model Chapter 7 contains information relating to GSIOC control and a list of available commands Hardware Description 333 and 334 Pumps are reciprocating piston pumps for preparative chromatography using from 20 mm to 100 mm bore columns Individually they are for single solvent delivery under high pressure Each 33X Pump is equipped with two pump heads 333 Pumps are master pumps designed to pump up to three solvents depending on the configuration They also have an integrated pressure purge and mixing module PPMM an outlet filter and optionally a solvent valve block 333 Pumps have
59. ate a Method Program using the control panel of the 333 Pump or from the controlling software For software information relating Gilson 15X Detectors you are advised to refer to the appropriate 15X Detector User s Guide 3 1 Installation Electrical Connections Switching on 333 Pump 334 Pump 3 Electrical Connections Switching On Power Supply Plug the power supply cord that you received with the pump into the socket on the power receptacle and to a suitable source of power The actual plug used depends on the country in which you will operate the pump should the one supplied not be suitable contact your Gilson representative Fuse Installation and Voltage Selection There are no fuses to install the pump is simply connected to an AC power supply of 110 120 V or 220 240 V Automatic selection of the operating voltage takes place on the power supply board Switching on Gilson 333 and 334 Pumps have two ON OFF switches one on the power receptacle and the other at the front above the LEDs To switch on a 333 or 334 Pump 1 Press the switch on the power receptacle to the T position the Power LED green on the front panel should light up if it does not check the power connections 2 Press the soft touch key on the standby panel the ON LED yellow should light up With a 333 Pump the start up screen should be visible on the control panel s display unit The third indicator light
60. ation m 0 means piston seal counter for head counter m 1 means piston counter for head counter m 2 means outlet check valve counter for head counter m 3 means inlet check valve counter for head counter x R means RESET counter x 0 to 65534 means set counter limit The limit value is in hours except for solvent selector valve where the limit is in 10000 cycles unit Command Cn m only sets the counter index used by the C immediate command N sduind ree pue geg 10 spuewwog GSIOC Commands for 333 and 334 Pumps 7 12 Command Type Description Cc l Read maintenance counters Response format is n m xxx yyy ZZZ n is the Head identification See buffered C command m is the counter identification See buffered C command xxx is the lifetime counter value in hours Does not exist for solvent selector valve counter yyy is the cycles counter value in unit 10000 cycles zzz is the counter limit value In hours for all counters except for solvent selector valve counter for the solvent selector valve the limit is in 10000 cycles unit The pump returns the counter with the index sets by the last buffered C command D B Dims or brightens front panel display Syntax Dn where n 0 dims display n 1 brightens display D l Read file directory Response format returns all existing file number separated by a comma If there is no existing file return N example 1 5 21 24 E B As
61. atthe for anew pump the Configuration Screen 50 appropriate point shows 333 as the model H3 as the head type Injection from pump NO Maximum number of solvents ONE to add solvent pump B press Hard Screen 78 appears at Extra solvent id 2 press Change until you see 334 or 333 press ENTER the Configuration Screen 50 should now show 333 as the model H3 as the head type Injection from pump NO Maximum number of solvents TWO then for each solvent pump if head type does not match those fitted to either pump select Head type press Change until you see the head type fitted H3 press ENTER 3 20 oO Installation dn bulyias Outlet Outlet Tee Inlet Tee Solvent A Pump ID 1 Solvent B Pump ID 2 or 3 Alternatively provided the first step 1 is completed correctly you may press Scan to identify any connected pumps which are then added to Screen 78 next to their currently configured IDs You are now ready to create your Method Program file s Optionally you can modify advanced configuration features refer to Chapter 4 3 Make the following hydraulic connections from the Outlet Filter of the Master 333 Pump to the downstream injector solvent line A to the inlet Tee piece on the Master 333 Pump solvent line B to the inlet Tee piece on the Slave 334 Pump s
62. autozero and detector lamp off Procedure 1 Make sure the Detector ID is set to 16 top switch and that the Baud rate is set to External bottom switch at position 0 2 Connect a GSIOC cable from the To Slave socket on your 333 Pump to the appropriate socket on the detector 3 Switch on both the pump and the detector at their rear panels 4 Switch on the pump and the detector lamp at their front panels Power and Lamp On 5 Wait 1 minute while the detector completes its validation process the top line of the pump s screen shows the status and after validation of the output from the active channel s 6 Press the Detect soft key on the pump Software Software Functions After pressing the Detect soft key on the pump a series of screens showing the pump parameters are available In addition you have access to the same soft key functions that are normally accessible from the control panels of the Model 151 and Model 155 detectors The soft keys are Next to access the following screen Previous to access the previous screen Mode to access mode and other soft keys Event to output an event marker Zero to zero the baseline The following parameters can be viewed sensitivity for each channel peak width ratio multiplier dual wavelength mode ratio threshold dual wavelength mode After pressing Mode the following soft keys become available Single to select single wav
63. ay d Screen contrast e Units of displayed values for flow rate pressure and injection volume Screen 50 Configuration Model 333 H3 Injection from Pe YES Controlled pumps 33X H3 33X H3 30X 10 Maximum number of solvents THREE Configuration Model 333 H3 Injection from pump YES Controlled pumps 33X 33X 30X 10 Maximum number of solvents THREE Safety 1 0 Misc Change Hard Hyd Screen 75 GSioc unite en nit id ENTER Bit rate 91 Turn etn SPAY after Omin s sine Ose eerie ast al arrow _keys _ iscellaneous Si0c unit ide Bit rate 19200 3 Turn off display after 0 min Screen display contrast Se naene use Change Units Changing the GSIOC ID The available soft keys are Units to modify the units displayed Screen 80 Change to change the current selection Key in a number between 0 and 63 then press ENTER Changing the Bit Rate 1 With the cursor at Bit rate press Change 2 At the required option EXTERNAL 1200 2400 4800 9600 19200 press ENTER EXTERNAL is the recommended setting 3 Press ESC once to return to Screen 50 A Software Changing the Screen Saver 1 Place the cursor at Turn off display after min 2 Key in a number between 0 and 999 minutes then press ENTER Bunu The display is turned off at the end of the specified period of time counting from the moment when you last pressed
64. ce Information 6 1 Reference Information Technical Data 6 2 1 The bias of a measuring 2 instrument is the systematic error of the indication of a measuring instrument The bias is normally estimated by averaging the error of indication over an appropriate number of repeated measurements source Characteristics of Measuring Instruments in International Vocabulary of Basic and General Terms in Metrology 2 Edition ISO 1993 Section 5 Gilson Operational Qualification procedure for 333 and 334 Pumps based on P A Hartman Proposed Standard Practice for the Evaluation of Gradient HPLC Pumps ASTM E 19 09 07 May 1990 Technical Data The following information presents construction and operational characteristics for Gilson 333 and 334 Pumps The operational characteristics include e Performance data quantifying separately the accuracy bias 1 and the associated repeatability Standard Deviation SD for pressure flow rate two solvent composition 2 and repeated sample injection from an extra pump These performance data were estimated for common solvents water methanol acetonitrile tetrahydrofuran isopropanol hexane and dichloromethane 20 23 988 1038 hPa 45 75 humidity over the whole nominal ranges for flow rate and pressure using the recommended values for adjustment parameters inlet pressure solvent name or compressibility correction and excluding the uncert
65. ces For example 7 75 min is actually 7 minutes and 45 seconds Units and Conversion Factors International System of Units SI SI units are used in this document for specifications and reference data although Units in Use with the SI Unit e g bar and liter are used in appropriate contexts The following information comes from the Handbook of Chemistry and Physics 79 edition by D R Lide CRC Press 1998 1999 Section 1 19 23 Name Symbol and Conversion factors Pressure Derived Unit Name of the SI Unit pascal symbol Pa Unit in Use with the SI Unit bar symbol bar Thermodynamic Temperature Base Unit Name of the SI Unit kelvin symbol K T K T 273 T T F 32 1 8 T F 1 8 x T C 32 Length Base Unit Name of the SI Unit meter symbol m 1 m 3 28 feet 39 4 inches 1 foot 30 5 cm 1 inch 25 4 mm Introduction Volume Derived Unit Name of the SI Unit cubic meter symbol m Unit in Use Together with the SI liter symbol liter lor L 1 liter 1 dm 1000 cm 1 gallon UK liquid 4 55 liter 1 gallon USA liquid 3 79 liter Weight Base Unit Name of the SI Unit kilogram symbol kg 1 kg 2 20 pounds 1 pound 0 454 kg Prefixes Prefix symbols should be printed in roman type upright with no space between the prefix and the unit symbol e g km for kilometer Prefixes are not to be used with temperature units
66. channe Operate output contacts 1 5 MPa Sample Screen 26 Solvent valve blocks Solvent A valve block A1 selected Solvent B valve block B2 selected Solvent C valve block C3 selected 4 19 Software Manual Operations 4 20 Screen 1 Screen 8 Screen 20 Screen 21 Back to Screen 20 at end of specified Ramping Time or after pressing End pump continues at flow rate and composition of Screen 21 Screen 1 Screen 27 The pulse length 0 01 to 1 minute is configurable Config I O Contact Pulse Duration Ne a Programming Manual Flow 1 Starting at Screen 20 key in a value for Ramping time 0 to 9999 minutes press ENTER 2 At the next line key in a value for flow 0 to 15 ml min press ENTER 3 At Composition key in a value 0 to 100 for B press ENTER 4 Repeat for C if present 5 Press Start to initiate pumping or ESC to abort and return to Screen 8 Output Refer to Chapter 3 for a physical description of the output connectors which may be programmed to send a signal to other equipment during a run Press Output you see the Operate Output Contacts screen Screen 27 for contact 1 to 4 the available soft keys are Open to set the contact to normally open Close to set the contact to normally closed Pulse to change the state open or closed of the contact 1 Press either of the horizontal arrow keys to select a
67. ched to a clip by pushing it gently into the fissure then the clip is pushed into the appropriate slot on the tray 7 Prime the solvent lines refer to Chapter 4 Installation Hydraulic Connections 3 10 Rinsing Line to Bottle Purge Line Rinsing Chamber Piston Rinsing Chamber If the solvent is an aqueous solution containing more than 0 1 M of solute which is solid in ambient conditions then the piston should be rinsed continuously with water A plumbing kit ref E66379 should be installed for the piston rinsing chambers of both heads 1 The plumbing kit consists of two rinsing lines which connect to the rinsing chamber inlets at the bottom of each head the longer line connects to the left head and two shaped purge lines which connect to the rinsing chamber outlets at the top of each head 2 Fill the glass bottle reference E66386 with distilled water and push the open end of each rinsing line through the bottle s pierced cap to between 1 to 2 cm of the bottom 3 Clip the rinsing lines to the tray Each line is first attached to a clip by pushing it gently into the fissure and then the clip is pushed into a slot on the tray 4 Ensure that each purge line is closed turn each connector fully counterclockwise until finger tight then press Manual Prime Start After about 20 seconds water should have sufficiently filled the rinsing line even though some air is also present 5 Press
68. commands unlike buffered commands allow the slaves to send data to the master Therefore status requests from the master must be immediate commands Connections between devices are made with specific Gilson GSIOC cables 9 pin D connectors The multi drop protocol allows the addition of more slaves into the system by permitting the cabling to be connected as a daisy chain GSIOC Physical Level 7 2 Physical Level GSIOC Control Cable The control cable contains one male and one female connector at the master end and one female connector at the slave end 770 mm Male Female Female GSIOC Connector Pin Functions The GSIOC cable has nine wires connecting corresponding pins GSIOC consists of three differential signal pairs the master data pair the slave data pair and the clock pair To improve immunity to electrical noise differential signals are used to eliminate ground loops in the system The pin out and pin functions are as follows Pin Function Source 1 Reserved 6 Reserved 2 slave data slave 7 slave data slave 3 master data master 8 master data master 4 clock master 9 clock master 5 ground N GSIOC Electrical Level The signals on the GSIOC are differential and are compatible with RS 422 and RS 485 specifications The master device drives both the master data pair and the clock pair J9A97 1 211 2913 Each slave drives the slave pair only whe
69. composition of the mobile phase WAIT to wait for a signal e g injection on input 2 OTHER to schedule a switch Solvent Valve Block event or a detector event OUTPUT to schedule output signals INJ to schedule an injection from the pump if configured A Software Creating a New File Editing an Old File Screen 1 Screen 1 Screen 2 Screen 2 sweibojg poya Huaug Screen 30 Screen 30 Screen 39 Screen 35 e Select You can enter all or any of these event types according to the requirements of your Method Program see Method Program work sheet page 4 29 Whichever event types you enter the procedure is the same 1 Press an event type key FLOW WAIT COMP etc you see the first File xxxx events screen Screen 36 the possible soft keys are Delete to remove an event from a file Present provided at least one event is present Create Add to create the first event in a new file or the first event of this type in an existing file Time Flow to toggle between injection flow rate and duration Add Create to add an event to a file List to review the events currently present in a file Select to choose an event type to add to the file Screen 39 Confirm to affirm the value entered at Screen 36a 2 Press Create or Add you see the second File xxxx events screen Screen 36a key in the time of the event followed by parameters which vary according to the even
70. compressibility as given in Chapter 6 Alternatively you can manually key in a value for compressibility see below Configuring Screen 90 Screen 96 Solvent A Select solvent A1 Head type H3 Solvent valve block A1 selected SOF RORANOE ER METHANOL HEXANE WATER DICHLOROMETHANE A4 WATER OTHER Solvent A1 water methanol Select the nearest composition 40 60 50 50 60 40 1 Starting at Screen 90 or Screen 91 solvent B or Screen 92 solvent C use the arrow keys to move the cursor to the channel or solvent then press Change 2 To select another solvent Screen 96 use the arrow keys to move the cursor to the required solvent then press ENTER You are returned to Screen 90 91 or 92 where the new solvent name should appear for the selected channel or pump 3 Starting at Screen 96 press HYDRO ORGANIC use the arrow keys to move the cursor to the required mixture then press ENTER Screen 98 lists water methanol mixtures and Screen 100 lists water acetonitrile mixtures use Next and Prev to switch between these screens 4 To enter a value for compressibility manually start at Screen 96 use the arrow keys to move the cursor to OTHER then press ENTER You are returned to Screen 90 where the solvent name is replaced by a compressibility value corresponding to the last configured solvent default value The moving cursor should be underneath the default value To enter a different value key in th
71. contact 2 Use the appropriate soft key to change the selected contacts state 3 Press ESC to return to Screen 8 A Software Entering Method Programs Creating and editing Method Program files is detailed in the following Sections You are advised to check and correct the configuration parameters before using the edit functions to create a list of events and the related parameters flow rates volumes composition and so on Creating a Method Program consists of two simple steps assigning a file number and entering a list of events that you want to occur at the times that you specify However it is recommended that you list the events required by your Method Program on paper before attempting to create the file sweiboig poya Huaug Method Program files 1 to 20 can be looped and linked to other files Safety Program files 21 to 24 are created in exactly the same way as Method Program files Getting Started Switch on the Model 333 Pump then after initialization you see the in run screen Screen 1 You will see the following soft keys at one time or another Pump Edit to access pump operations Detect to access an associated detector Manual to prime and operate manually Run to run the current Method Program file Pause to interrupt the Method Program Resume to restart a paused Method Program End to stop a Method Program Stop to stop pumping Zero to zero the detector signal if associated
72. cratic work GLP functions audit trail of unexpected events anomalies conditional operations loops and links maintenance logs for all wear parts use and limits hours and number of cycles automatic procedures for piston seal installation leak test and mixing test Data transfer PC software supplied on diskette permits to view and print with headlines all method files application safety and mixing test plus configuration and audit trail 605 interface required Windows 95 98 or NT Time range from 0 01 to 9999 min 0 6 s to 166 h by steps of 0 01 to 1 min according to the range used Loops 1 999 default 1 Link one for each file default none Adjustment Parameters Ramping time for manual flow control 0 9999 min default 0 min Head size H3 6 7 Reference Information Technical Data Compressibility correction K 0 2000 Mbar default 34 Mbar for water Inlet pressure P 0 20 MPa default 0 MPa Initialize piston before injection from pump yes or no default no After power failure continue stop or start a specific file default continue Pause input contact with or without flow default without flow Wait for injection input contact close or open no default compulsory answer depending on associated injector Output contact state close open or pulse no default compulsory answer depending on associated instrument Pulse output contact 0 01 1 mi
73. d Parameters are ASCII codes as follows Code Keyname Code Key name Comment when this command 7 ai has been sent the keyboard is a Okey ja rake locked but i b Softkey F2 T One ocked but it can memorized up to Softkey F3 2 Two 8 key strokes beep can be heard d SoftkeyF4 3 Three The key codes are stored ina e SoftkeyFS 4 Four buffer At the time the keyboard is T SoftkeyF6 S Rive reconnect to the software the 2 joar 2 en f 7 E Enter 7 Seven buffer is cleared Dec point 8 Eight Command K without any codes xX Escape 3 Nne reconnects the keypad to the u p TA E TEA internal software D Downarrow R Right arrow Command K merely locks the keypad Comment The message Keypad locked is shown on the lower line of the display instead label of soft key For the remote pumps the remote led is turned on when the keypad lock command K is received It is turned off with the unlock command K GSIOC Command Type Description K l Read key entry Response format x xx where x xx is an ASCII string up to 8 characters long encoding the last keys pressed This command clears the buffer Comment If no key pressed the ASCII characters is returned If the keyboard has not been disconnected by a buffered command k the
74. d flow rate the duration is calculated according to the volume of sample you specify and vice versa Flow rate and volume depend on the size of head fitted to the 30X Pump There are two extra soft keys Screens 35 and 36 for an injection event Time Flow to select time as the third parameter Flow Time to select flow rate as the third parameter 1 Key in the time at which the injection starts 0 00 to 9999 minutes then press ENTER 2 Key in the volume of sample to be injected 0 to 500 ml then press ENTER 3 Key in an injection flow rate 0 001 to 5 ml minute then press ENTER or 4 Key in an injection duration 001 to 9999 minutes then press ENTER 5 Press Confirm to affirm the values entered 6 Press ESC to go back to Screen 30 OTHER After pressing OTHER you see Screen 40 for solvent selection press Solvent for a detector event press Detect Solvent 1 Key in a time 0 00 to 9999 minutes then press ENTER 2 Press Change to select from the available channels A1 to A4 B1 to B4 C1 to C4 3 Press ENTER then Confirm 4 Press ESC to go back to Screen 30 or Prev Detect 1 Press Lamp off or Zero 2 Key in a time 0 00 to 9999 minutes 3 Press ENTER then Confirm 4 Press ESC to go back to Screen 30 or Prev A Software Creating Loops You create loops to repeat the Method Program n times which means the number of times the Method Program will be exec
75. ds the state of the physical input Read contact input buffer Response format same as immediate command Comment this command reads the input buffer of the internal software instead of the physical input N sduind pee pue geg 10 spuewwog 7 19 GSIOC Commands for 333 and 334 Pumps 7 20 Command Type Description J B Write contact outputs Syntax Jabcd where a is the Out1 relay b is the Out2 relay c is the Outs relay d is the Out4 relay Parameters C for Close D for Open P for Pulse X for state unchanged for reconnect to internal software Comment This command disconnects the output from the internal software if the corresponding parameter is C D or P The default pulse duration is 0 03 min unless set otherwise by the buffered command E J l Read contact outputs Response format abcd as buffered J command for each output C if closed and connects to internal software c if closed and disconnects from internal software D if open and connects to internal software d if open and disconnects from internal software The returned state s refers to the physical output s j l Read contact output buffers Response format and parameters same as immediate J command K B Input remote keystrokes Syntax K key codes up to 32 key codes per comman
76. dth of min ranging from 0 to 999999 p1 to p3 are additional parameters depending on event type The meaning and number of parameters depends one event type see below When an event is added it is sorted by increasing time order and event type If the application is full the new eventis ignored Parameter Minimum Maximum Event type 0 FLOW EVENT pi Flow 1 10 pl min 5 for 32X See F command 40 for 333 Event type 1 MIXTURE EVENT pi Percentage of pump B in 0 1000 and p1 p2 p3 inferior or equal to 1000 p2 Percentage of pump Cin 0 1000 and p1 p2 p3 inferior or equal to 1000 p3 Percentage of pump Din 0 1000 and p1 p2 p3 inferior or equal to 1000 Event type 2 OUTPUT EVENT p1 Output number 1 4 p2 Outputstate 0 CLOSE 1 OPEN 2 PULSE Event type 3 INJECTION EVENT p1 Injection flow 1 10 l min See min and max flow for the injection pump p2 Injection volume 1 10 ul See min and max volume for the injection pump Event type 5 WAIT EVENT p1 Input state 0 wait input close 1 wait input opened GSIOC Command Type Description G Read application event from Edit file Returns event selected by application event index as previously set by a buffered G command Response format EventNb Type Time p1 p2 p3 where EventNb range from 0 to 29 Other parameters separated by a comma are defined in buffered G command Note Type 255 means empty event End of file
77. e required compressibility and then press ENTER 4 12 Software A Safety Functions Press Safety you see the Pressure Limits screen which shows the high and low pressure limits and the associated safety files The available soft keys are Next to configure Screen 50 the Other safety i m er functions Screen 33X 65 RR SE eects ence Prev to return to the Pressure Limits screen Pressure limits Screen 66 High 28 0 MPa starts file 21 Configuration Model 333 H3 Injection from pump Controlled pumps 33X H3 33X H3 30X 10 Maximum number of solvents THRE Safety 1 0 Misc Change Hard Hyd Screen 65 Change to change Low 00 0 MPa starts file 22 ESC the current selection Screen 66 Other safety functions Other safety functions nen poe restored after failure u power restored after failure tart file 23 ut 2 close starts file 24 n 2 close starts file 24 nction starts beeper alarm YES Pressure Limits are model and configuration dependent and subject to automated validation You need to ensure that the pressure limits defined here are suitable for the safe and correct operation of your system Other safety functions allow you to decide on the course of action after a power failure and to turn on or off the beeper Take care to ensure that safety files started as a result of choices made here perform the desired actions e g stop pumping
78. e Information 6 26 GSIOC T GSIOC stands for Gilson Serial Input Output Channel GSIOC is a bidirectional communications channel that can link a controlling device with up to 63 other devices The system controller or master module controls all of the connected devices or slaves in the system by sending GSIOC commands The master communicates with one slave at a time When the master identifies a slave it connects to the channel as the previous slave disconnects Each device connected to the GSIOC channel is distinguished by a unique GSIOC identity number ID For the 333 Pump the ID may be set to any number between 0 and 63 for the 334 Pump the ID may be set from 0 to 9 333 and 334 Pumps can receive GSIOC commands as can most other Gilson modules 333 Pumps are also capable of sending commands as the controlling device Alternatively the controlling device may be a computer via a suitable interface on which a GSIOC driver and the controlling software is installed The controlling software must be able to receive and transmit GSIOC commands character by character according to the protocol specified in this document There are two command types that the controlling device sends to a slave device buffered and immediate The slave executes buffered commands as background processes Immediate commands have a higher priority the slave device interrupts the execution of a buffered command to execute an immediate command Immediate
79. e and Troubleshooting 5 For 333 and 334 Pumps user maintenance is generally limited to the following 1 cleaning check valves and filters 2 replacing parts subject to wear and tear in each pump head piston seal check valves and piston assembly General guidelines for the periodic replacement of the wear parts are indicated below according to the amount of use intensive regular or occasional This schedule should be regarded as a guide changes in performance or visible leaks give an indication that a part should be changed Typical Replacement Schedule for Wear Parts Component Intensive 168 h week Regular 40 h week Occasional 10 h week Piston seals 4 5 months 3000 h 1 1 5 years 2500 h 2 years 1000 h Check valves 7 months 4500 h 1 5 years 3000 h 3 years 1500 h Piston assembly 9 months 6000 h 2 3 years 5000 h 4 years 2000 h The figures are based on the assumption that the pump is working at half its maximum flow rate and pressure The nature of the liquid pumped is a major factor affecting longevity of the piston seal e standard UHMWPE seals are best suited for water aqueous solutions alcohols acetonitrile and in general polar solvents e black PTFE piston seals offered as additional accessories are best suited for tetrahydrofuran hexane methylene chloride carbon dioxide and in general low polarity solvents You can check and reset your pump s Mai
80. e efficiently Change the inlet filter if you suspect that it has become plugged Outlet Filter The outlet filter protects the injection valve and the column A plugged outlet filter may cause pressure build up and leaks You should routinely check and clean the interior of the outlet filter and when necessary replace the filter cartridge 1 Remove the filter from the pump 2 Separate the two halves of the filter casing using two 11 mm wrenches and remove the filter cartridge 3 Rinse the interior of both halves of the casing using a suitable solvent using an air line to complete the cleaning process 4 Clean the filter cartridge using a jet of solvent or fit a new filter cartridge 5 When you reinstall the filter cartridge place it in the black downstream half of the casing this ensures that the cartridge is properly seated before reassembling the filter casing 6 Reassemble the filter casing using moderate force then refit the filter to the pump and re prime the system checking for leaks Maintenance and Troubleshooting Troubleshooting When troubleshooting try to check each part of the system independently try one solution at a time and proceed in a systematic way If for example the delivered flow rate is not correct check each pump head independently Check the solvent bottles the connections between the bottles and pump heads inlet filters outlet filters and so on Systematically ch
81. e requirements of the receiving device b An output pin 9 is available on the right hand socket for feeding a recorder or a PC via a suitable interface This output which comes from the pump s microprocessor can be configured to follow pressure flow or composition A B or C It is labelled Digital but outputs a series of discrete signals 0 1 V via the digital to analog converter c An output pin 10 is available on the right hand socket for feeding any suitable recorder or a PC via a suitable interface This analog output which comes directly from the sensor is for pressure only 0 142 1 V for 0 60 MPa Input Signals Four pairs of terminals of the right hand socket are dedicated to specific software related input functions START END PAUSE RESUME INPUT WAIT Input 1 EMERGENCY Input 2 Installation You connect a pair of wires from an output e g relay type of the external device to a pair of terminals for each of the functions that you want controlled externally Except for WAIT to activate one of these inputs you must change the state close or open of an output on the external device START END An external relay contact connected to this input may be used to start OPEN gt CLOSE and stop CLOSE gt OPEN program PAUSE RESUME An external relay contact connected to this input may be used to pause OPEN gt CLOSE and resume OPEN gt CLOSE the Method
82. eck each component in the circuit even if it s new Refer to the following tables for diagnostic information relating respectively to electrical and to hydraulic problems Error situations are signalled by a 333 Pump by means of an error message appearing on the screen and the error LED on the front panel lighting up On the 334 Pump the error LED is replaced by remote this LED simply indicates when the slave is being controlled from the master Error LED 333 Pump The error LED could light up steady red for any of the following reasons 1 A pump motor has ceased to function or has been asked to function in a way that is not possible 2 Communication has failed with a slave pump 3 Pressure limits have been exceeded high file 21 or low file 22 Any attempt to run a file that does not exist will activate the error LED 4 Restart after a power failure has attempted to start file 23 However the file does not exist the soft ware stopped the pump and activated the error LED 5 Input 2 was closed attempting to start file 23 However the file does not exist the software stopped the pump and activated the error LED 6 A maintenance counter limit has been reached see Chapter 4 7 The audit trail is saturated 8 Invalid setting O1 BHuljooysajqnol Maintenance and Troubleshooting Troubleshooting Error Messages 333 Pump Many types of messages are displayed on the screen for e
83. ed with a 333 Pump not shown in most of the Figures given in this Chapter 2 For the functions accessible from the Detect soft key you should refer to the user s guide for the relevant detector A Bunu 4 7 Software Configuring 4 8 Screen 50 Configuration Model 333 H3 Injection from pump NO Maximum number of solvents ONE Screen 78 Hardware Configuration Model 333 H3 Controlled pumps for Extra solvent id2 NONE Scan checks the ids of the controlled pumps which must be connected via GSIOC and switched on Scan does not validate the pump s configuration you must ensure that you describe the pump correctly to the software Hardware Configuration Starting at Screen 50 which shows the current configuration press Hard you see the Hardware Configuration screen Screen 78 The available soft keys are Change to change the current selection Scan to check the GSIOC bus for suitably connected and viable pumps Configuration Model 333 H3 Controlled pump 33X Injection from pump NO Maximum number of solvents TWO A Master 333 Pump can control one or two additional solvent pump Slaves and an injection pump The controlled pumps must be assigned as follows Extra solvent id 2 can be a 333 Pump or a 334 Pump Extra solvent id 3 can be a 333 Pump or a 334 Pump Injection id 4 must be a 30X Pump if an injection sample pump is pr
84. ed from experiments to maximize the flow rate accuracy i e minimize the bias minimize its pressure Solvent K Mbar dependence center it on zero and obtain closely Water 34 related values for common solvents having very Methanol 162 different physical properties Extensive measurements Acente 180 of the bias versus X were carried out over the whole pressure range Isopropanol 162 Ethanol 148 For Gilson 333 and 334 Pumps the empirical Tetrahydrofuran 150 compressibility correction K maximizes the accuracy Hexane 290 of flow rate and two solvent composition over the Heptane 270 whole of their nominal ranges for flow rate and Bichloromathane 200 Pee Chloroform 204 Empirical Compressibility Correction K Mixture K Mbar Mixture K Mbar Water methanol 10 90 130 Water acetonitrile 10 90 146 Water methanol 20 80 110 Water acetonitrile 20 80 123 Water methanol 30 70 92 Water acetonitrile 30 70 103 Water methanol 40 60 73 Water acetonitrile 40 60 82 Water methanol 50 50 55 Water acetonitrile 50 50 62 Water methanol 60 40 46 Water acetonitrile 60 40 52 Water methanol 70 30 43 Water acetonitrile 70 30 48 Water methanol 80 20 40 Water acetonitrile 80 20 42 Water methanol 90 10 37 Water acetonitrile 90 10 36 Le Aoeinooy ayey MOJ4 Reference Information Properties of Common Solvents Properties of Common Solvents With reference to the table lines 1 to 8 a
85. ee Table amp notes 116 R W L Injection pump liquid See Table amp notes 120 RL Postrun information file number 1 to 24 or 0 if none selected 121 RL Post run information recorded 1 recorded 0 not rec d 122 RL Post run information maximum pressure 1 10 MPa see pressure limits 123 RL Post run information minimum pressure 1 10 MPa see pressure limits 124 RL Post run information cycle time solvent A 1 100 min 1 to 99999 0 n a 125 RL Post run information cycle time solvent B 1 100 min 1 to 99999 0 n a 126 RL Post run information cycle time solvent C 1 100 min 1 to 99999 0 n a 127 to 129 Reserved 130 R W L Pump A selector A1 Liquid Compressibility X Mbar 0 to 2000 see notes 131 R W L Pump A selector A2 Liquid Compressibility X Mbar 0 to 2000 see notes 132 R W L Pump A selector A3 Liquid Compressibility X Mbar 0 to 2000 see notes 133 R W L Pump A selector A4 Liquid Compressibility X Mbar 0 to 2000 see notes 134 R W L Pump B selector B1 Liquid Compressibility X Mbar 0 to 2000 see notes 135 R W L Pump B selector B2 Liquid Compressibility X Mbar 0 to 2000 see notes 136 R W L Pump B selector B3 Liquid Compressibility X Mbar 0 to 2000 see notes 137 R W L Pump B selector B4 Liquid Compressibility X Mbar 0 to 2000 see notes 138 R W L Pump C selector C1 Liquid Compressibility X Mbar 0 to 2000 see notes 139 R W
86. elength mode Dual to select dual wavelength mode Scan to store a reference scan or to compare with previous reference File to access the file functions Setup to configure the detector Status to view and reset lamp usage etc For more information refer to the 151 or 155 Detector User s guide A For all 15X detectors the remote indicator lights up after pressing the Detect key on the pump s control panel plus pressing a detector command e g Zero after which for the 151 and 155 Detectors selections made from the pump s control panel are shown on its screen and are mimicked on the detector s screen Under remote control the 151 and 155 keyboards no longer function 4 45 10 99 8q XSL I PON L JO 101 U09 Software PC Software for 333 and 334 Pump Control 4 46 PC Software for 333 and 334 Pump Control Users of Gilson s UniPoint software who want to control or communicate with 333 or 334 Pumps should refer to the corresponding user s guide for further information GSIOC commands may also be used to dismount and remount pump heads and to read modify or reset the maintenance counters 1 Use the GSIOC Utility Software installed with UniPoint including the following dialog boxes Identification Number Command Immediate or Buffered and Response 2 Enter GSIOC commands and parameters corresponding to the desired information in the appropriate dialog boxes Maintenanc
87. ellows to be slid back into position f d Inserting the Tool e Opening the Orifice f Refitting Step 1 ee O1 aoueUs UIEWY pedyH dung 5 5 Maintenance and Troubleshooting 5 Pump Head Maintenance Pull on the metallic ring to refit 2 Pull on the metallic ring at the end of the bellows the bellows moderate force is i until it can go no further g required When refitting the 8 8 bellows support the pistonby 3 Remove the tool and check that end of the Menedd Norbyhe shart bellows with the metallic ring is correctly seated against the piston collar h g Refitting Step 2 g Refitting Step 3 Metallic Ring Reassembling a Pump Head 1 Push together the two halves rinsing and pumping chambers of the pump head with a slight twisting motion 2 Turn the rinsing chamber relative to the pumping chamber until holes for the pump head retaining screws are aligned because of the asymmetry of the holes there is only one correct position 3 Check that the marks on the rinsing and pumping chambers are aligned a 4 Refit the bellows new if necessary to a clean piston and insert the assembly fully into the rinsing chamber b a Correct Alignment of Chambers and Pistons b Correctly Piston Assembly Cotter Pin amp Alignment Marks eee Maintenance and Troubleshooting 5 Turn the piston until the small cotter pin at the rounded end of the piston is in line approximat
88. ely with the alignment marks on the pump head 6 Refit the white cap c reinsert the screws and progressively tighten them d making sure that the alignment marks are still correctly aligned do not overtighten the screws c Refitting the White Cap Do not turn the piston after the head is reassembled because it is possible to damage the bellows d Tightening the Screws O1 aoueUd UIEWy pesyH dung Maintenance and Troubleshooting 5 Check Valves The inlet and outlet check valve cartridges are identical for H3 heads but the connectors are not take care Check Valves The two check valves inlet and outlet should be cleaned periodically to ensure reliable flow rates If they become partially blocked the flow rate will drop in which case they must be cleaned or replaced For 333 and 334 Pumps Gilson check valves are supplied in the form of cartridges one for the inlet connector and one for the outlet connector Cleaning a Check Valve This procedure is carried out with the check valves in situ 1 Open the purge valve to the drain position 2 Pump isopropanol provided the current solvent and isopropanol are miscible 3 When the pump head is full of isopropanol stop the flow for at least 15 minutes to dissolve any sticky deposits 4 Reconnect the current solvent and pump to the drain to clear the isopropanol 5 Check that the flow rate has returned to normal if not remove the check va
89. en run and when there is no associated 15X Detector Screen 1 looks like this when you switch on and a Method Program file has been run previously Screen 1 may look like this where at the end of the Method Program the flow rate is gt zero A dund 34 UO BulysyiMms Screen 0 333 H3 Version 1 00 Initializing Screen 1 0 00350 AU at 254 nm Pump file 11 000 ml min 0 A 0 B Pump Detect Manual Detector file 1 0 0 MPa Screen 1 Pump file 000 ml min Screen 1 Pump file 12 Loop 1 000 ml min 498 ml min 95 0 A 5 0 B Convention for pump file numbers Pump file no file selected Pump file xx file xx is selected but is empty Pump file xx file contains at least one event Method Program or Safety File 4 3 Software Priming Priming The following steps must be completed before operating the pump under the control of the pump s software by a computer based program or manually from the pump s control panel 1 Make the electrical and hydraulic connections to the pump s 2 Connect the power and switch on the pump s 3 Prime the hydraulics initialize and run in the piston seals if new Hydraulic Priming This is an essential step which must be carried out before operating a 333 Pump or 334 Pump 1 If one or more pumps are controlled from a 333 Pump the additional pump s must be declared in the configuration see Conf
90. erence Information Technical Data 6 6 Control Characteristics Control from a 333 Pump Control Panel Keypad 25 functional keys including six soft keys Display eight lines of 40 characters each adjustable contrast 10 position turning off after 0 999 min default 10 min Keystroke beeper on or off default on Alarm beeper on or off default on Controlled Gilson Instruments Gilson 333 GSIOC master can control a Gilson detector and 3 other Gilson pumps For UV vis absorbance detection a single wavelength model 151 152 or a dual wavelength model 155 156 Forrepeated sample injection into preparative systems a 30X Pump 305 306 307 308 with any head For up to three solvents two additional 33X Pumps For up to three solvents and repeated sample injection two additional 33X Pumps plus one 30X Coordination with any other instrument carried out by electrical contacts Electrical Contacts Maximum accepted voltage 48 V for each input and output contact Inputs TTL type wait for injection configurable and programmable emergency signal run end and pause resume Outputs four configurable and programmable outputs relay type 30 V 2 A one DC power supply 12 V 0 5 A to be associated with a programmable output one digital output converted into analog signal 1 V pin 9 and configurable for pressure flow rate or composition one analog output 142 1000 mV pin 10 for
91. esent Adding a Solvent Pump 1 Use the arrow keys to move the cursor to Extra solvent id 2 if you want to add an extra pump for solvent B and then to Extra solvent id 3 for solvent C If you only have two solvent pumps the second pump must be configured as solvent B 2 Press Change until you find the required option 333 or 334 then press ENTER or press Scan to scan the GSIOC bus for devices connected to the pump 3 Press ESC to return to Screen 50 check that all pumps are listed correctly including the head type for 30X pumps e g 33X for 333 and 334 30X 10 for 305 306 307 and 308 or NONE A Software Adding an Injection Pump 1 Use the arrow keys to move the cursor to Injection id 4 to assign a 30X Pump for injecting samples 2 Press Change to select 30X then press ENTER or press Scan to scan the GSIOC bus for devices connected to the 333 Pump 3 Press ESC to return to Screen 50 check that the injection pump is listed correctly the format for a 30X Pump is 30X abc where abc is the configured pump head size see Hydraulic Configuration You must confirm the assignment as follows with the cursor at Injection from pump NO press Change until you see YES then press ENTER Bunu Removing a Pump 1 Use the arrow keys to move the cursor to Extra solvent id 2 if you want to remove the extra pump for solvent B 2 Press Change unt
92. et must be unique for each item of Gilson equipment For a 333 Pump the ID 0 63 is configured as follows 1 Switch on the pump wait until initialized 2 Press in turn Edit Config Misc 3 Key in the desired ID for the 333 Pump then press ENTER For a 334 Pump the ID 0 9 is set mechanically using the left hand of the two selectors on the rear panel see Figure 3 5b For a 305 Pump the ID 0 63 is configured using the 305 Pump s keypad see 305 Pump User s Guide For a 306 Pump the ID 0 63 is set mechanically using switches on the rear panel see 306 Pump User s Guide Bit Rate You must use the default values for a system where a 333 Pump Master is controlling other devices slaves When a 334 Pump is used as a slave to a 333 Pump the bit rate of the slave must be set to External Or when the bit rates of the sending and receiving devices need to be matched you can set a specific bit rate oO SUOI JEDSIUNWIWOYD SUOI DOUUOD e9293 3 7 Installation Electrical Connections Communications GSIOC ID 0 9 333 Pump ID 1 From Controller 334 Pump ID 2 From Controller Bit Rate 0 External 1 9600 baud 2 19200 baud 333 Pump ID 1 334 Pump ID 2 From Controller For a 333 Pump the bit rate is set as follows 1 Switch on the pump wait until initialized 2 Press in turn Edit Config Misc 3 Press the down arrow key 4 Press Chan
93. first line N sduind pee pue geg 10 spuewwog 7 23 GSIOC Commands for 333 and 334 Pumps 7 24 Command Type Description U Delete Audit Trail file Syntax U Write display Syntax Wm xx xx Where m line number 0 to n 1 n being the number of the line xx XX is an alphanumeric string up to 40 characters long Note that characters shown on the display unit may differ from characters sent by a computer The string is made of letters A Z a z numbers 0 9 special characters amp and space If the string is less than 43 characters 3 40 the remaining right most characters of the display are blanked If it is longer extra characters are ignored The vertical bar is not required if this command is the last one in the buffer This command disconnects the corresponding line from the internal software The syntax has several variants W0 xx x disconnects and writes xx x on line 1 Wn xx x disconnects and writes xx x on line n 1 W disconnects the whole display but lines are not blanked WO disconnects line 1 but lines are not blanked Wn disconnects line n 1 but lines are not blanked W reconnects all lines Wo0 reconnects line 1 Wn reconnects line n 1 Read display Response format Wn xx xx Where nis the line number 0 to 7 xx XX is a 40 character alphanumeric string This command returns the contents of the
94. for an immediate command response N EWIO4 pue 3497 194981849 7 5 GSIOC Disconnect and Connect Sequences 7 6 Disconnect all Slaves Delay 20 ms Send Unit ID Code no 20 ms Timeout 2 yes Error Handler Sy Sele T Disconnectand Connect Sequences The following sequence is used to select a slave device 1 The master sends a 255 ASCII character FF hexa decimal to disconnect all slaves from the GSIOC 2 The master device uses one of the following terminations to ensure that no slaves are active passive no break termination the master waits for 20 milliseconds to allow all slaves to disconnect break active the master receives a break character as soon as a selected slave disconnects 3 The master announces the binary name of the desired slave device The value of the binary name is equal to the unit ID plus 128 10000000 binary For example if a unit s ID is 16 10000 binary its binary name is 10010000 Binary names are used to identify devices because GSIOC interprets unit IDs ASCII 0 to 63 as commands 4 The slave device that recognizes the binary name as its own connects its transmitter to the slave data channel and echoes its binary name to the master The selected slave device must respond within 20 milliseconds otherwise the master assumes that the desired slave is not available Any slave device that does not recognize it
95. from 2 2 0 1 ml at 2 ml min to 3 7 0 1 ml at 200 ml min pressure independent Effective mixing vol indicative of mixing volume 2 from 1 2 0 1 ml at 2 ml min to 2 7 0 1 ml at 200 ml min Composition time constant to reach the injection valve with 63 of the nominal composition value from 40 s at 2 ml min to 1 s at 200 ml min Gradient linearity range 2 1 98 B for 10 ml min and higher Accuracy bias lt 0 7 B from 10 composition steps for 10 ml min and higher Repeatability SD lt 0 5 from 2 composition steps for 10 ml min and higher Residual UV absorbance pulsation amplitude for binary mixtures lt 2 of the UV absorbance contrast between the two solvents or 10 mAU cm whichever is the greater Sample Injection from Extra Pump Requirement extra Gilson 30X pump 305 306 307 308 with any head tee fitting and extra tubing at column inlet Volume range from 2 x 10 to 10 x head size in ml 10 pl to 20 liters Flow rate from 2 x 10 to 1 x size in ml min 10 pl min to 200 ml min Minimum adjustments 10 x head size for volume ml and flow rate ml min Time from 0 01 to 9999 min Injection volume accuracy bias lt 1 or5x 10 x head size in ml whichever is greater for the whole volume range Injection volume repeatability SD lt 0 5 or 2 x 10 x head size in ml whichever is greater for the whole volume range 6 5 Le eed jed1UYyoeL Ref
96. ge until you see the desired bit rate 1200 to 19200 or External 5 Press ENTER For a 334 Pump the bit rate 9600 19200 or External is set mechanically using the right hand of the two selectors on the rear panel When a 334 Pump is used as a slave to a 333 Pump you must select External For a 306 Pump the bit rate is set mechanically using switches on the rear panel see 306 Pump User s Guide When the 306 Pump is used as a slave to a 333 Pump you must select External External clock control should also be selected for all pumps running under computer control Internal is used when the connected device does not provide a clock source in which case you have to select an appropriate bit rate Twin Pump Systems Two pumps may be connected in parallel thereby doubling the programmed flow rate In theory there is no limit to the number of pumps that can be connected in parallel but the twin system with two liquid streams is the most practical The hydraulic outlet tubings are connected together using a Tee piece to increase the overall flow rate To set up 333 or 334 Pumps to operate in parallel you must give each of the paralleled pumps the same GSIOC ID the Master 333 Pump has an ID 1 as does its twin the Slave 32X Pump and its twin both have an ID 2 and so on The twinned pumps are connected together using GSIOC cables When operating a twinned system the commands from the controlling device g
97. gth of an output pulse to between 0 01 and 1 minute 0 6 to 60 seconds c You may set the output signal to follow pressure flow rate composition A B or C If you choose one of the composition parameters you should also enter a value for Delay Volume 0 to 90 ml to get the best synchronization between the programmed profile and the detected profile Changing a Function 1 With the cursor at Input pause press Change 2 At the required option WITH FLOW WITHOUT FLOW press ENTER 3 With the cursor at Contact pulse duration key in a value 0 01 to 1 press ENTER 4 With the cursor at Analog output signal press Change 5 At the required option FLOW PRESSURE A B or C press ENTER 6 If either A B or C is selected Delay Volume appears next line With the cursor at Delay Volume key in a value 0 and 90 press ENTER 7 Press ESC to return to Screen 50 4 15 Software GSIOC ID and Miscellaneous 5 Press Misc you see the Miscellaneous screen Screen 5 75 which allows you to modify the following items O 4 16 a GSIOC id 0 63 This must be done if one 333 Pump is to be used as a slave to another each must have a unique id or if the default id 1 conflicts with other equipment b Bit rate of the 333 Pump External 1200 2400 4800 9600 19200 c Turn off the display after x minutes press any key to reactivate the displ
98. hases with high pressure mixing binary systems require two pumps 333 334 ternary systems require three pumps 333 334 334 Composition flow rate and events including solvent switching if SVB is fitted are all programmable from the 333 Pump or from a PC using Gilson software UniPoint Working Range and Performance Data Solvents Nature common solvents buffers and any liquids chemically compatible with the flow path materials see below Viscosity 0 3 20 mPa s cP Temperature 2 40 C Compressibility up to 2000 Mbar Solute concentration typically up to 1 M of solutes being solid in ambient conditions piston rinsing chamber is a standard feature pH 1 13 if less than 0 1 M chloride ions Flow path Materials Metals stainless steel AISI 316L and titanium ASTM grade 2 Thermoplastics FEP PTFE PCTFE ETFE and UHMWPE Refractories pump head ruby and ceramics Pressure Nominal range from 0 5 MPa 5 bar 70 psi up to 21 MPa 210 bar 3040 psi Selectable units MPa bar and psi default MPa three significant digits Reference Information Technical Data Readout increment 0 1 MPa 1 bar 10 psi Digital output acquisition period 500 1000 ms pin 9 Analog output 142 1000 mV for 0 60 MPa pin 10 Safety limits low and high both adjustable from 0 to 21 MPa default 0 and 21 MPa Accuracy bias lt 2 or 0 1 MPa whichever is greater Repeatability
99. he 334 Pump at the right you require a special shaped tubing ref E66360 Solvent B is routed via the outlet tee piece of 334 Pump to an inlet on the PPMM of the 333 Pump where the two solvents are mixed at high pressure The 333 Pump can be stacked on top of the 334 Pump in which case you must use the connecting tubing for vertical stacking reference E66451 Outlet et Tee Heads Inlet Tee Solvent A Solvent B Pump ID 1 Pump ID 2 or 3 GSIOC Cable Gilson Interface 506C Setting up What You Must Do 1 The two pumps must have different GSIOC IDs except if working in parallel normally 1 and 2 Set their GSIOC IDs using the rotary switches on their rear panel 2 Make the electrical connections between the PC systems interface module The two female connectors on the GSIOC cable are plugged into the FROM CONTROLLER sockets on the pumps and a second cable connects from the male socket to the next unit in the line e g 15X Detector or the systems interface module Gilson 506C 3 Switch on the pumps 4 Use the controlling software UniPoint to configure and program the pumps 3 24 oO Installation 5 Make the following hydraulic connections from the Outlet Filter of the 333 Pump to the downstre
100. he next device Thus you can daisy chain the pumps and other Gilson equipment such as a 15X Detector A A 334 or a second 333 Pump is being controlled from a 333 Pump Plug one end of a GSIOC cable into the socket marked GSIOC FROM CONTROLLER on the first pump or detector being controlled and plug the other end into the socket marked GSIOC TO SLAVE on the controlling pump B A 334 or 333 Pump is being controlled from a computer Plug one end of a GSIOC cable into the socket marked GSIOC FROM CONTROLLER on the first pump being controlled plug the other end into the GSIOC socket of a Gilson 506C System Interface Module and connect an RS232 cable from the 506C to the computer Alternatively you can use a Gilson 605 RS232C GSIOC Adapter Chapter 7 contains a description of the GSIOC cable connector pin out information a detailed description of the GSIOC protocol and a list of commands Installation GSIOC ID You must use the default values for a system where a 333 Pump Master is controlling other devices slaves By default the master pump is assigned ID 1 the slave elution pumps are assigned ID 2 and 3 The slave injection pump is assigned ID 4 The GSIOC IDs may be changed where the pump s are being controlled from a computer In which case the configured IDs must correspond to those set using the controlling software For each level the GSIOC identification number ID that you s
101. hod Program file Edit Create or View to modify an existing Method Program file View Edit or Create to review an existing Method Program file Delete to delete the currently selected file Lock Unlock to lock or unlock the currently selected file Copy to copy the currently selected file Links shows which files are linked to the currently selected file juowabeuey aj Create or Edit These keys allow you to create a Method Program in a previously empty file or to edit an existing file View View enables you to view a locked file using the same screens as Edit but without the possibility to use the Delete key to remove events from the file currently selected or to delete the file itself However you may copy a locked file and then edit the copied file Delete To delete a file press Delete Screen 18 then press Yes If in doubt press No because a deleted file cannot be recovered unless a copy exists Pressing either key returns you to Screen 11 Lock To lock a file press Lock Screen 19 then press Yes If in doubt press No a locked file cannot be edited or deleted However you may copy a locked file in which case the copy is automatically unlocked by the software A locked file is indicated by an asterisk before the file number Pressing either key returns you to Screen 11 4 31 Software File Management 4 32 UnLock To unlock a file press Unlock Screen 19 then press Yes
102. iguring 2 Fill the solvent bottles with degassed HPLC grade solvents and immerse the filters of the pumps inlet tubings in these bottles 3 Switch the valve to the purge position 4 Press Manual Prime then Start for the pump head that is to be primed see Manual Operations If after two minutes solvent does not flow from the purge valve s outlet check that the valve is in the open position then remove the tubing and attach a syringe to the purge valve s outlet using a suitable adapter 5 Draw solvent into the syringe while continuing to pump When solvent appears in the syringe press Stop to cease pumping 6 Reconnect the tubing and continue priming for as long as is necessary No bubbles should be present in the solvent flowing through the tubing Press Stop to cease pumping 7 Repeat the procedure for the other pumps in the system Software A Running a pump head dry for more than a short time will damage the piston seal B Ensure that the purge valve is fitted with a drain tube before priming the pump C During priming the low pressure limit is inactive the high pressure limit is automatically set to 3 MPa to protect the column if you forget to open the purge valve in which case the screen displays the following message Open Purge Valve After Priming 1 Use the GLP function Seal to initialize the piston seals 2 After completing the installation and configurati
103. il you find the required option NONE then press ENTER 3 With the cursor at the appropriate line repeat for Extra solvent id 3 or repeat for Injection id 4 Press ESC to return to Screen 50 Hydraulic Configuration Press Hyd to access the Hydraulic Configuration screens for each of the solvent pumps defined earlier The first Screen 90 is for Pump 1 Solvent A the second Screen 91 is for Pump 2 Solvent B and the third Screen 92 is for Pump 3 Solvent C You move between screens using the Next Prev keys The sample pump is accessed using the Inject soft key Each screen enables you to select the head type define a Solvent Valve Block SVB and name a solvent for each of its four channels or to specify a value for compressibility for each The available soft keys are Next to go the next screen Prev to go to the previous screen Adjust to configure advanced hydraulic functions Software 4 Configuring 4 10 Change to change the current selection Inject to configure the sample injection pump Configuring a Solvent Pump For each solvent pump 1 Check that the head corresponds to the type fitted press Change to modify the type configured press ENTER to confirm For 333 and 334 Pumps the head type must be H3 2 For each pump fitted with a SVB use the arrow keys to select Solvent valve block NONE press Change to select a solvent channel A1 to A4 B1 to B4 C1 to C4
104. ing to the channel s you wish to prime Self priming is generally obtained after 2 minutes If not press Stop Disconnect the drain tubing from the purge valve and replace it with a suitable syringe equipped with its adapter Press Start then draw on the syringe piston while the pump is active 3 When the line is filled with liquid press the Stop soft key corresponding to the channel s you wish to stop priming 4 Press ESC to return to Screen 8 You must stop all channels before pressing ESC in order to leave this screen Running a pump head dry for more than a short time will damage the piston seal Therefore be prepared to intervene manually in the priming process Manual Flow Control Press Flow you see the Manual Flow Control screen Screen 20 after entering the parameters the available soft keys are Start to start pumping after ramping on to the desired flow rate and composition Present if the values demanded are different from the actual values Stop to stop pumping immediately Present only if flow is not equal to zero End to interrupt the ramp on Screen 21 pumping continues Zero to zero the detector signal if associated Screen 20 is the ready to run screen which displays dynamic data for the pump and an associated detector top line A Screen 1 Pump file ji 00 ml min A 0 B Screen 8 suo1 1 3do jenuen Manual control Condition or ee flow s Prime
105. ion Pump 1 Starting at Screen 50 press Hyd to access the configuration screen for solvent A Screen 90 2 At Screen 90 or Screen 91 solvent B or Screen 92 solvent C press Inject to access the parameters for the injection pump Screen 94 Refill Time Inlet Pressure Head Type Compressibility Refill Time 125 1000 ms is the duration of the piston return stroke If cavitation occurs use a higher value Compressibility 0 2000 Mbar 1 is the compensation parameter for solvent compressibility 3 Use the arrow keys to move the cursor to the parameter that you want to change 4 Key in the desired value then after keying in the value press ENTER After pressing ENTER the cursor jumps automatically to the next parameter In particular you must key in an appropriate see above value for compressibility Screen 50 Configuration Model 333 H3 Controlled pump 33X Injection from pump YES Maximum number of solvents TWO Screen 90 Screen 94 Solvent A Injection Head type H3 Refill time 125 ms Solvent valve block ATRE Inlet pressure 0 0 MPa 2 W Head type eo Compressibility 34 Mbar1 A Buun uos Software 4 Named Solvents Compressibility For each solvent channel A1 to A4 B1 to B4 or C1 to C4 or pump A B or C you can select a solvent from the list of names or press HYDRO ORGANIC to select from the list of mixtures The software will automatically enter a value for
106. ion flow rate F is calculated as a function of five variables F f Fy Vy Vo P X where V is the volume of the dead space inside the compression chamber P is the operating pressure X is the compressibility of the liquid under the pressure P In the software X is calculated using the simplified Tait equation X c P d Coefficient c varies only slightly with the nature of the liquid It is a constant included in the software Coefficient d is calculated first estimate from liquid compressibility at atmospheric pressure X for P 0 Values of X for some common solvents are given in the following tables The operating pressure P is continuously transmitted by the Pressure Transducer to the firmware in the pump Reference Information 3 The complementary compensation flow rate F is defined as the difference F F F F When F was measured experimental results yielded a simple function F f a b P Coefficients a and b were determined for each pump head they are manufacturing constants related to the pump head size Adjustments Experimental results showed that it was possible to define an optimum empirical value K for X This value K called empirical compressibility correction for use with Gilson 32X and 33X Pumps is given below Your attention is drawn to the fact that K is not a physical constant The empirical values generated at 20 23 C were obtain
107. ion linearity range 2 97 B Composition accuracy bias lt 1 B for each composition step Composition repeatability RSD lt 1 Environmental Conditions Operation Voltage 90 260 V 50 or 60 Hz Power 600 W Electrical installation category II Temperature 10 40 C for 333 Pump 4 40 for 334 Pump Humidity 15 80 Pollution degree 2 Storage Temperature 15 TC to 40 Humidity as for operation Size and Weight 333 Pump Width 260 mm height 507 mm depth 410 mm Weight gt 35 kg 44 kg packed 334 Pump Width 260 mm height 387 mm depth 410 mm Weight gt 35 kg 44 kg packed Reference Information Le Solvent Miscibility Miscibility means that solvents should mix with each other in all proportions That solvents should e miscible is important both during elution and when switching from one solvent to another io AYIIQIOSIIN JUBAJOS You are advised to refer to the table below when selecting solvents For some solvents lower toxicity alternatives are indicated 1 2 3 as follows oO 1 Dichloromethane oOo 2 Tetrahydrofuran 000 ener Bomac OOOO ooon O00000 CYCLOHEXANE LJ OOO DICHLOROETHANE w O000000 DICHLOROMETHANE O0O00000og0 DIMETHYLFORMAMIDE TOO OOOOOO Dnem suFOXDE_ OOOOOmoOooo Pokna Cd J OOOOOBOOOOO eTHYLACETATE DOO OOOOOOOOO ETHANOL CU J OO OOOOOOOOOOo DFETHYLETHER TOO OOOOOOSOOOO HEPTANE O0DmMOC COCCCOCAHMO0OCOOO HE
108. ional Qualification procedure 333 and 334 Pumps 1 801397 Unpacking notice 1 E66382 PC software for 333 Pump data transfer 1 e2 6 21 SIOQUINN Hed Reference Information Part Numbers 6 22 Gilson 334 Pump Reference Description E66014 334 Pump 110 and 220 V single solvent 200 ml min 21 MPa Gilson 334 Pumps can accept any electrical voltage from 90 to 260 V 50 or 60 Hz Each is supplied with two power cords part number 500006 for 110 V and 500005 for 220 V Standard accessories Reference Description Quantity Hydraulic 866149 Bottle tray for 333 and 334 Pumps 1 E66381 Inlet tubing FEP 3 2 x 4 8 x 1250 mm 3 16 with filter for connecting to pump tee piece 1 E66379 Plumbing kit for piston rinsing chambers connect to pump heads 1 E66386 Bottle glass 180 ml pierced PE cap screwed cap for piston rinsing solvent 1 E66360 Tubing 316 steel 2 1 x 3 2 x 600 mm 1 8 2 08 ml pre shaped 334 tee to 333 PPMM 1 Mechanical 610101 Spanner for tubing nuts 6 3 7 9 mm 4 5 16 1 610112 Spanner for check valve holder 14 mm 1 610117 Spanner for outlet filter double ended 11 and 13 mm 2 610043 Allen wrench 3 mm rear end to release pump head 1 610045 Allen wrench 5 mm front end to remove pump head 1 E66157 Tubing clip PP for 3 2 mm 1 8 for 333 and 334 Pump bottle tray 2 E66158 Tubing clip PP for 4 8 mm 3 16 for 333 and 334 Pum
109. ith drain tubing silicone 4 x 6 x 1000 mm 33X Pumps 420028 Tubing silicone 4 x 6 mm per meter drip pan drain E66463 OQ plumbing line fully equipped 333 and 334 Pumps includes 1 x 430060 Tubing 316 steel 0 25 x 1 6 x 550 mm 1 x 410426 Nut 316 steel 10 32 TPI 1 6 mm 1 16 tubing 1 x 410425 Ferrule 316 steel 10 32 TPI 1 6 mm 1 16 tubing 1 x 410456 Union fitting 316 steel 10 32 TPI 0 025 ul Upchurch U435 430060 Tubing 316 steel 0 25 x 1 6 x 550 mm 410426 Nut 316 steel 10 32 TPI 1 6 mm 1 16 tubing 410425 Ferrule 316 steel 10 32 TPI 1 6 mm 1 16 tubing 410456 Union fitting 316 steel 10 32 TPI 0 25 mm through 0 025 ul Upchurch U435 E66357 Tubing 316 steel 2 1 x 3 2 x 210 mm 727 ul preshaped 2 fittings PPMM to outlet filter E66450 Tubing 316 steel 2 1 x 3 2 x 600 mm 2 08 ml preshaped 2 fittings 333 tee fitting to PPMM E66355 Tubing 316 steel 2 1 x 3 2 x 197 mm 682 ul preshaped 2 fittings right H3 33X to tee fitting E66356 Tubing 316 steel 2 1 x 3 2 x 197 mm 682 ul preshaped 2 fittings left H3 33X to tee fitting E66360 Tubing 316 steel 2 1 x 3 2 x 600 mm 2 08 ml preshaped 2 fittings 334 tee fitting to PPMM E66314 Tee fitting 316 steel 1 4 28 TPI 2 1 mm through 38 ul 866028 H3 Pump Head for 333 and 334 Pumps Reference Information Reference Description 866344 PPMM 316 steel and PTFE 30 MPa 2 85 ml 333 Pump 410707 Filter assemb
110. ization you see the ready to run screen Screen 1 You will see the following soft keys at one time or another Pump Edit to access pump operations Detect to access an associated detector Manual to prime and operate manually Run to run the current Method Program file Pause to interrupt the Method Program Resume to restart a paused Method Program End to stop a Method Program Stop to stop pumping Zero to zero the detector signal if associated 1 Press Pump Edit you see the Pump Control screen Screen 2 you may be presented with the following soft keys at one time or another File to access the file management operations Edit Create or View to modify an existing Method Program file Create Edit or View to enter a new Method Program file View Edit or Create to review an existing Method Program file Config to enter a configuration parameters for the currently selected file GLP to access audit maintenance run in and test functions for a 333 Pump Watch to obtain post run information 2 Press File to access the file management screen you see the File Directory screen Screen 11 which shows all currently assigned files Use any of the arrow keys to move around the screen Which of the possible soft keys you see depends on the state of the file you select A Software file unedited empty file locked file linked Create Edit or View to enter a new Met
111. le Command reads the audit trail file selected by the index sets with the buffered O command which must be used before o l Read Audit Trail files events See G Command for response format Returns event selected by Audit Trail file event index This command increments automatically the Audit Trail file event index This index is reset by the O buffered command which must be used before N sduind pee pue geg 10 spuewwog 7 21 GSIOC Commands for 333 and 334 Pumps 7 22 Command Type Description Q B Enter pressure value Syntax Qbxxx in bar Qpxx xin MPa or Qkx xx in kpsi If the parameter xxx is omitted only the GSIOC pressure unit used in immediate Q command is changed This command does not affect the pressure unit for the user interface Comment This command disconnects the pressure value from the internal pressure transducer Q reconnects pressure to the internal pressure transducer Q l Read pressure value Response format as above in the pressure unit used by the last buffered Q command The default unit is the bar S l Buffer status Response format ab where a 0 if the GSIOC buffered command buffer is empty a 1 otherwise b 0 if all buffered commands have been accepted since the last immediate S command b 1 if one or more buffered command has been rejected since the last immediate S command b is reset to 0 after it has been t
112. lows Four arrow keys to navigate around the screen Eleven numeric keys 0 to 9 and to enter values for predefined parameters ENTER to enter a value or option into memory HELP for detailed help messages including the screen number CLEAR to cancel a value before it is entered into the memory ESC to change from a software level to a higher one Software Switching On the Pump 1 The power supply switch located on the rear panel must be set to the ON position I the POWER LED comes on Next press the ON OFF switch on the standby panel at the front of the pump the ON LED illuminates 2 After switching on a 333 Pump the display shows Screen 0 for one second whilst initialization takes place During which time a message indicating the software version is displayed then you see the ready to run screen Screen 1 This dynamic screen varies according to the associated equipment whether a Method Program exists and according to in run information Wait for 1 second Screen 1 looks like this the first time you switch on when a Gilson Model 15X Detector is associated with the pump In this case the top line is dedicated to showing the output signal and wavelength of that detector Dual wavelength detectors 155 amp 156 have both output signals displayed The Detect key accesses the detector functions Screen 1 looks like this the first time you switch on when no Method Program file has yet be
113. lve 6 Clean the check valve by blowing compressed air though it or replace it with a new one Maintenance and Troubleshooting Replacing a Check Valve You can if necessary replace a check valve without dismounting the head However in this case you must first turn off the pump and disconnect the hydraulic tubing s from the connector s 1 Loosen the connector using the supplied 14 mm wrench 2 Fully unscrew the connector from the pump head by hand 3 Remove the check valve from the connector 4 Make sure that the connector and pump head housing are clean 5 Slide a new check valve with the orientation shown in the figure into the connector 6 Screw the connector into the pump head housing 7 Carefully tighten the connector using a torque wrench set to 7 Nm Or turn the connector using the 14 mm wrench until there is contact then tighten the connector by turning it a further 30 in the clockwise direction If leakage is observed tighten the connector progressively until the leakage stops 8 Run the pump and perform the leak test Chapter 4 Check Valve H3 Arrow on the H3 inlet an outlet cartridges must point in direction of solvent flow O1 S AJLA 42949 Maintenance and Troubleshooting 5 Filters Filters Inlet Filters To protect the check valves an inlet filter must be used with all solvents Inlet filters must be in good condition for the pump to operat
114. lvent Inlet Check Valve Pump Heads H3 pump heads for preparative use flow rates between 0 20 and 200 ml minute 21 MPa are pre mounted directly onto the tops of the driving mechanisms which have the same axis as the piston motors so pump heads may be serviced with relative ease The pump heads must be dismounted for routine servicing purposes e g changing a piston seal Each head has a solvent inlet port a solvent outlet port an inlet port to the rinsing chamber an outlet port from the rinsing chamber and a reciprocating piston Shown here are the external components the internal components are described in Chapter 5 Maintenance The piston seal and the bellows are inside the pump head The solvent inlet port and the solvent outlet port are fitted with connectors containing the check valves All of these items can be serviced by the user Description Optional Components Solvent Valve Block Up to four solvent lines may be connected to the solvent block of each configured 333 or 334 Pump These solvents may be switched under software control Thus a two solvent workstation where each pump is equipped in this way permits selection of solvents A1 to A4 from Pump A and B1 to B4 from Pump B Adding a third pump enables you to select solvents C1 to C4 Solvent Degasser The Gilson 864 Degasser is an on line solvent degasser with four channels operating under a vacuum of 70 hPa It maximizes the stability of the
115. ly 316 steel 2 1 mm thru 10 um 1 6 x 19 mm 21 MPa 333 Pump Upchurch 1579 410730 Filter 316 steel 10 um 1 6 x 19 mm 333 pump Upchurch A331 E66391 Tubing 316 steel 2 1 x 3 2 x 500 mm 1 73 ml straight to injector 430057 Tubing 316 steel 1 x 1 6 x 600 mm 471 ul straight to injector E66394 Tubing 316 steel 0 13 x 1 6 x 185 mm 2 ul preshaped one fitting GLP Seal E66384 Adapter 316 steel 1 4 28 TPI male and 10 32 TPI female 1 mm through 11 ul 410470 Nut 316 steel 1 4 28TPI for 3 2 mm 1 8 tubing Upchurch C235 410471 Ferrule 316 steel for 3 2 mm 1 8 tubing Upchurch C236 410478 Plug 316 steel 1 4 28 TPI 333 and 334 Pumps Mechanical and Electrical E66211 Column holder clips 1 4 two units E66212 Column holder clips 1 2 two units E66215 Column holder clips 1 two units E66157 Tubing clip PP for 3 2 mm 1 8 tubing and 33X bottle tray two units E66158 Tubing clip PP for 4 8 mm 3 16 tubing and 33X bottle tray 500933 GSIOC Cable 506341 Barrier strip connector 14 pin output contacts 506367 Barrier strip connector 10 pin input contacts and two outputs Documents and Data Transfer Software 801422 User s guide 333 and 334 Pumps 804040 Installation Qualification procedure 333 and 334 Pumps 804041 Operational Qualification procedure 333 and 334 Pumps E66382 PC software for 333 Pump data transfer e2 6 25 SIOQUINN Hed Referenc
116. m from detector and to collection vessels 6 x 410428 Nut POM white 1 4 28 TPI for 3 2 mm tubing Upchurch P303 6 x 410429 Inverted ferrule ETFE natural for 3 2 mm tubing Upchurch P300N 1 x 410153 Coupling PVDF 1 4 28 TPI E66451 Tubing 316 steel 2 1 x 3 2 x 663 mm 2 30 ml pre shaped 334 tee fitting to PPMM vertical stacking 430067 Tubing 316 steel 1 x 1 6 x 900 mm 1 16 707 ul system connections 430046 Tubing 316 steel 2 1 x 3 2 x 2000 mm 1 8 6 9 ml system connections Mechanical and Electrical E66195 Valve holder without valve E66197 Column holder equipped for 2 to 20 mm i d column for 333 and 334 Pumps E66201 Shelf 180 x 240 x 425 mm external for stacking pump or injector over detector 500944 Cable kit 4 wire 1 7 m for electrical input output contacts Wear Parts All wear parts are hydraulic parts Reference Description 410730 Filter 316 steel 10 um 1 6 x 19 mm for 333 and 334 Pumps Upchurch A331 400140 Piston seal UHMWPE yellow flange type Ti spring for H3 pump head 400141 Piston seal PTFE black flange type Hastelloy C276 spring for H3 pump head E66330 Check valve cartridge inlet and outlet for H3 pump head E66333 Piston assembly for H3 pump head e2 SIOQUINN Hed 6 23 Reference Information Part Numbers 6 24 Replacement Parts Reference Description Hydraulic 866383 Valve block 4 solvent without holder and tubing
117. men sur 3 14 Postanite the Auti SE 200000070000000000000000000000000000000000000000000000 00a 3 15 HonzontalContigurationm a 3 15 Vertical Stackine e E ncevsivare 3 16 Seting Up mee cues E E E E E E 3 17 Basic Elements m e e tnea nen eee ears 3 17 Config Example 1 Binary Gradient or Isocratic 3 19 Config Example 2 Solvent Mixing and Injection 3 22 Config Example 3 333 334 Pumping System with Control from a PC 3 24 sine the ContrelPanel ues mania meen e eunnnce 4 2 Display Umit m a creer tear ats 4 2 Keypad eae e E 4 2 pwitchite OFN ne PUNY 20000250200000000000000008000050090079007300900290990903090000 4 3 EMINE a aa a e E a 4 4 Vey ine D0 Fela etal b ug hg sae oarne eave areca e eoee ty Pau cranrrec rane yst 4 4 Aften Priming eea ea arsesctvonnmnerssunaescs 4 5 CONCreaS so Oba a miami seen siat 4 6 Introduction e R 4 6 Procedure ee e are ee eee eee 4 6 Table of Contents 2 IMlatd Wate CCN ptitaOnssgsrancc ue sect cman 4 8 Hydraulic Conte tration 20000000000000000000000000000000000800000000030000000 4 9 Safety Functions eee ahacn ea ntnrncmceatians 4 13 Blechrical Ontactsi ccs tesserae eters 4 15 CSODA WiscellaneGusr ss ceeee erasers 4 16 Mantial perations o2000200000008000000000000000000600070000009900900007306000000000000 4 18 Introduction ee se ete ecne eee eee 4 18 Procedure seen ia se A cetecesscenretesteeoe oeenrteremttos ace 4 18 Hydraulic Priming e cerevisiae atenaer
118. million cycles The parts logged are the piston piston seal inlet check valve In CV outlet check valve Out CV After the specified usage you would normally service or replace the part in question see Chapter 5 You specify limit values that are suitable for your applications and in line with GLP procedures applicable to your working environment 1 After selecting a pump head press Logs 2 To reset a logged value use the vertical arrow keys to select the part press Reset 3 To change an upper limit use the arrow keys to select the required field key in the new value then press ENTER The flashing cursor indicates the currently selected field 4 Press two times ESC to return to Screen 82 AN A suonoun 9919814 10 e10qe pooy 4 35 Software Good Laboratory Practice Functions 4 36 Seal Installation This procedure is designed for installing new piston seals using isopropanol For a different solvent you should adapt the flow rate in proportion to the viscosity of the solvent used The procedure is in two parts first priming for two minutes at a fixed flow rate to the drain see table below second pumping at a pre programmed gradient ascending then descending flow rate against the back pressure provided by the supplied capillary tubing for 14 minutes If the pressure indicated inthe table is reached before 2 minutes then the software interrupts the positive flow rate
119. mn supports into either of the slots 2 Fix the column support in position using a knurled screw 3 Repeat for the second column support but don t fully tighten the screw 4 Slide the second column support along the long slot to match the length of the column 5 Fully tighten the screws Injection Valve Holder The injection valve holder has two pairs of holes one pair is for mounting the valve in the vertical position and the other is for mounting the valve in the horizontal position Holder Installation 1 Loosely fit the retaining studs to either pair of holes 2 Slide the feet into the top of the retaining slot at the side of the pump 3 When the holder is securely positioned fully tighten the retaining feet knobs Valve Installation 1 Secure the valve body to the holder using two screws 2 Fit the valve handle as described in the documentation supplied by the valve manufacturer OO sallosseo0y Installation Accessories 3 14 Solvent bottle Tray The figure shows the tray being fitted to a 333 Pump For a 334 Pump the tray simply sits on top of the pump its feet resting in the special recesses Installation Positioning the Pumps Horizontal Configuration In normal use the pumps may be placed side by side see Configuration Example 1 The 333 Pump Solvent A at the left is fitted with PPMM and outlet filter To connect to the 334 Pump at the right you req
120. n 3 The installation procedure you used 4 A concise list of the symptoms 5 A list of operating procedures and conditions you were using when the problem arose 6 A list of other devices connected to the system and a system diagram showing the connections 7 A list of other electrical connections in the room BIIAIBS JOWO SND Introduction 1 10 Description 2 The front of a 333 Pump incorporates the control panel and the pump s principal hydraulic components which are pre mounted The hydraulics may be concealed by the removable door Also shown is the standby panel which shows the operating status of the pump and may be used to switch on and off the pump The 334 Pump which is shorter has no control panel and operates in the slave mode There is a drip tray at the bottom of both pumps Solvent bottles can be placed in a removable tray at the top of a 333 or a 334 Pump on the bench or on the floor A single 333 Pump is for use in the isocratic mode By adding one or two 334 Pumps two or three solvents may be mixed By adding a 30X pump solvent injection may be performed However in total no more than three additional pumps of any type may be controlled from a 333 Pump whether the controlled pumps be used for mobile phase or for injection 2 1 Description 2 Standby Panel Control panel Standby Panel Solvent Tray Pump Heads Drip Tray Door Hydraulics Drip Tray Door 2 2 Description
121. n default 0 03 min Analog output profile pin 9 pressure B C or flow rate default pressure Delay volume associated with composition profile analog output 0 90 ml default 0 GSIOC unit identification 0 63 for 333 default 1 0 9 for 334 default 2 GSIOC bit rate external 19200 9600 4800 2400 or 1200 baud for 333 default external external 19200 or 9600 baud for 334 default external Parameters for Associated 30X Injection Pump Head size 5 10 25 50 100 or 200 default 5 Refill time 25 1000 ms default 125 Compressibility correction and inlet pressure as above Maintenance Counters Time up to 9999 h for wear parts piston seal check valves and piston assembly Cycles up to 10 for wear parts Computer Control of 333 and 334 Pumps From a future version of Gilson UniPoint system software via Gilson 506C interface and GSIOC slave bus From other system software using Gilson 506C or 605 interface GSIOC slave bus and commands refer to Chapter 7 e2 Reference Information Hydraulic Components Standard Components Low pressure Plumbing Filter 316 steel 20 um for 4 8 mm 3 16 tubing Tubing FEP 3 2 x 4 8 mm 3 16 Nut POM white 5 16 24 TPI for 4 8 mm 3 16 tubing Ferrule ETFE natural for 4 8 mm 3 16 tubing e eq jed1UYydeL H3 Piston Pump Heads Identification Gilson 866028 plus serial number Flow path materials 316 steel body ce
122. n connecting to a two pump system a GSIOC Cable is also required from the To Slave socket on the Master 333 Pump to the From Controller socket on the slave pump 2 Using a Gilson 506C Interface For more complex systems you need a Model 506C Interface a 9 pin D female to 25 pin D male converter a 25 pin male female connection cable i Connect the 9 pin female end of the converter to a 9 pin male RS 232 socket on the IBM PC ii Connect the female connector of the 25 pin cable to the 25 pin male connector on the converter iii Connect the male connector of the 25 pin cable to the RS 232 socket of the 506C Interface Software iv Connect a GSIOC cable from the GSIOC socket of the 506C Interface to the 333 or 334 Pump Installation 1 The PDT Software runs under Windows 95 or Windows NT 4 0 2 Place the diskette supplied by Gilson in drive A 3 Run the Setup exe file 4 Follow the instructions given on the screen Functionality Four data types can be transferred from the pump Audit Trail Method Configuration and Counters After transfer data can be printed or stored as files on the computer All files stored on the computer can be recovered and printed Two types can be transferred back to the pump Method and Configuration The table shows the functions that are possible for each data type You can add comments or supplementary information to each file saved Transferable
123. n it is selected All slaves must be capable of deselecting from the channel on command Both the controller and slaves should look for parity framing and overrun errors Although GSIOC is differential the common mode voltage between slaves and masters should be less than 7V to ground The ground connection is not implemented in every GSIOC device so they must be grounded locally by connecting the machine to a good earth circuit This ensures compliance with the common mode specification The GSIOC clock is either transmitted by the channel link external clock or its local internal clock in which case Master and Slave must have the same bit rate The clock runs at sixteen times the desired bit rate normally set at 19200 For a 333 Pump the bit rate may be set using the control panel to 1200 2400 4800 9600 19200 or External for a 334 Pump three switch setting are available 9600 19200 or External Bit Rates When a 333 Pump is used as a slave to another 333 Pump or is controlled from a computer the bit rate of the slave must be set to External Or when the bit rates of the sending and receiving devices need to be matched you can set a specific bit rate for both For a 333 Pump the bit rate is set as follows 1 Switch on the pump wait until initialized 2 Press in turn Edit Config Misc 3 Press the H key 4 Press Change until you see the desired bit rate 1200 to 19200 or External 5 Pres
124. n seal gt sequence m S to start sequence p the run in head 0 for heads of pump A 1 for heads of pump B 2 for heads of pump C 3 not used in this context 4 for the head of the inj pump q the flow rate used to reach the run in pressure in tenth of ul m C to continue sequence after priming see immediate e command n 1 gt Start lt Leakage test gt sequence m test pressure value in tenth of Mpa ranging from up to system maximum pressure p the flow rate used to reach the test pressure in tenth of ul n S gt Stop running maintenance sequence If m p q are not useful they do not exist calibrate pressure transducer Syntax cammm Where a L for low point calibration a H for high point calibration mmm is the calibration pressure in tenths of MPa 0 to 600 for the high point calibration It does not exist for low point calibration Pressure transducer calibration status Response format a Where a if there is no calibration before a Y if the previous calibration command was successful a N if the previous calibration command was unsuccessful Leakage maintenance sequence status Response format a Where a R for sequence running a K if last sequence was successful a F if last sequence failed a if no leakage sequence N sduind pee pue geg 10 spuewwog 7 25 GSIOC C
125. nal accessory Solvent B is routed via the outlet tee piece of 334 Pump to an inlet on the PPMM of the 333 Pump where the two solvents are mixed at high pressure The tubing linking the two pumps goes through the tubing port together with solvent and rinsing port tubings In the figures the tubing port is in the position where the tubings are locked in place To make it easy to install and to remove tubings there is a fissure in the tubing port which is accessed by rotating the tubing port until the fissure lines up with the opening in its housing oO Installation Setting up Basic Elements dn bulyias Take care when you are reconfiguring a 333 Pump and have previously created Method Program files you will probably need to modify these files if they are to work correctly with the new configuration types of solvent associated pumps etc A 333 Pump may be used alone or as the master pump controlling up to two other solvent pumps 333 or 334 It may also be used to command an injection pump 30X 334 Pumps are for use as extra solvent pumps always connected hydraulically to the PPMM of a 333 Pump Outlet Outlet Tee Heads Outlet Inlet Tee Solvent Inlet via 20 m filter Pump ID 2 or 3 Key PPMM See text below OF Outlet Filter Solvent Inlet T Tee piece via 20 m filter Pump ID 1 3 17 Installation Setting up 3 18
126. nce 0 for lt To run in new piston seal gt sequence running 1 for lt Leakage checking gt sequence running b is the pump status for normal operation L for low pressure limit the reading resets the low pressure limit state H for high pressure limit cis the invalid condition flag for normal operation F for invalid settings The invalid conditions flag is reset by Start a file or send a flow 0 using the buffered F command dis the status of the right head actuator in single piston mode or the status of both head actuators in Dual piston mode for no errors E if there is an error e is the status of the left head actuator in single piston mode for no errors or if the pump works in dual piston mode E if there is an error kkkkkkk Application control syntax is ab where a is S for Stop R for running application b is the running file number P for Pause Q for Resume application This command will be ignored if it is inconsistent e g run an application which does not exist Write maintenance counters Syntax is Cn m x where nis the Head identification n 1R means right head of master pump if 333 n 1L means left head of master pump if 333 n 2R means right head of slave pump 1 n 2L means left head of slave pump 1 n 3R means right head of slave pump 2 n 3L means left head of slave pump 2 m is the counter identific
127. ndersigned hereby declare that the equipment specified above conforms to the above Directives and Standards a Herv Le Dorze Quality Assurance Manager Place Sarcelles Issue Date 03 01 2000 The Gilson S A quality assurance system is registered as complying with ISO 9001 International Quality Standard Registration Certificates No 6621 and No 18623 BVQI Declaration of Conformity 1 Introduction 1 Gilson 333 and 334 single solvent pumps are for use in preparative chromatography 20 to 100 mm bore columns Described in this User s Guide they are individually known as 333 Pumps and 334 Pumps Also described is Gilson 333 334 as a gradient system Notational Conventions and Units Introduction Conversion Factors To Convert Multiply by from bar MPa psi atm 1 013 0 101 14 7 bar 0 987 1 0 1 14 5 MPa 10 1 145 psi 0 068 0 069 0 0069 1 1 atm 760 mm Hg 104 mm H O 1 hPa 1 mbar 10 mm H O 2 1 mm Hg 1 Torr 1 33 mbar 133 Pa 0 0193 psi Notational Conventions and Units Software Related Conventions 333 Pump The software displays messages and read only values on the control panel s screen as normal typeface inside a frame This convention is followed in this User s Guide For software options where a key must be pressed the related function is represented in bold e g Edit HELP When time is expressed in minutes it is to two decimal pla
128. ng from the GLP Screen 82 press Seal Screen 265 you will see these soft keys at one time or another Change to select the pump head to run in Start to start the pumping suonoun 39119e1g A10 e10qGe7 poos Continue to start pumping at the programmed rate End to stop the pump 1 Connect the supplied capillary tubing ref E66394 to the outlet of the outlet filter then switch the purge valve to the drain position 2 Press Change followed by ENTER to select the pump to run in 3 Optionally if you are not using isopropanol as the solvent you may change the flow rate Normally you should keep the default value given in the table 4 Press Start to start the pump Screen 266 or End to stop the pump in an emergency 5 After two minutes the pump stops Screen 267 switch the purge valve to the use position then press Continue 6 The pump then runs the pre programmed sequence Screen 268 7 After the program has finished Screen 265 press ESC Screen 82 then run the leak test or press Seal to repeat the procedure for another pump 4 37 Software Good Laboratory Practice Functions 4 38 The selected test pressure must be within the configured pressure limits Leak Test This test consists of pressurizing the pump at a user selectable pressure in a closed hydraulic circuit When this pressure is reached the pump stops If during the next 5 minutes the pressure decay is less than
129. nimum and the maximum pressures attained during the latest run of the file selected by the watch file number the time taken per cycle for each piston provided the flow and composition remained constant during the run This may be useful information when analyzing baseline pulsations for example In the case of linked files the first one is selected automatically but you can select another one For a complete log of events you should use the Audit trail function Audit trail records the unprogrammed events that take place during a run when you execute one or more Method Program files Audit trails are recoverable by PC based software Before a run of after pressing Stop no flow Pump file 19 Loop 1 0 ml min 0 A 0 B During a run flow and composition changing Pump file 19 Loop 1 3 1 58 7 5 min 4 2 ml min 25 A 75 B During a run after pressing Pause flow and composition constant at rates when program was paused Pump file 19 Loop 2 3 Pause 0 50 min 4 2 ml min 25 A 75 B During a run after pressing End flow and composition constant at rates when program was ended Pump file 19 Loop 2 1 50 min 7 0 ml min 16 A 84 B Manual Run Sto After a run before pressing Stop flow and composition constant at rates when program ended Pump file 19 Loop 3 10 0 ml min 50 A 50 B Manual Run Sto A weiboig poyan e Buluuny 4 41 Software
130. nt via Gilson 506C interface and GSIOC slave bus Coordination with any other instrument is carried out by electrical contacts One of the following Gilson detectors UV vis absorbance detection may also be controlled from a 333 Pump single wavelength Model 151 or 152 dual wavelength Model 155 or 156 You should refer to the user s guide of the relevant detector for full information including soft key functions that are accessible from the control panel of a 333 Pump Operating Principle You have to go through three main steps before running your 333 Pump based Method Program 1 Define the system configuration enter descriptions of your pumping system s hardware 2 Select the type of events and key in the related parameters flow rate composition and coordination The Method Program configuration list of events and associated parameters is saved automatically by the software 3 Initialize the system by priming the solvent channels then run the Method Program Introduction Unpacking Hardware You are advised to check your pump immediately even if it is not to be used until later Upon receipt of your instrument unpack the unit carefully inspect it for possible damage and check the contents of each carton against the list of parts and accessories given in the Chapter 6 Your supplier should be notified immediately of any inconsistencies or any damage Your pump is delivered in a crate containing the m
131. ntenance Logs press Edit GLP Maint If your type of use is intensive with relatively constant solvents and operating conditions then set the limiting values numbers of hours to reflect your experience as well as GLP requirements 5 1 Maintenance and Troubleshooting Pump Head Maintenance Pump Head Maintenance Before a head can be physically removed from a 333 or a 334 Pump you must disengage the pump head from the pump motor by using the software dismount procedure This procedure is accessed from the control panel of the Master 333 Pump or by GSIOC commands from the PC based controlling software see page 4 35 There is an alternative manual procedure in case of the loss or unavailability of power see below Normal Dismounting Procedure 1 Open the purge valve by turning the black knob on the Pressure Module counterclockwise 2 After powering up the pump use the software dismount procedure refer to Chapter 4 to release the pump head 3 Disconnect all solvent lines from the pump head s in question 4 Progressively remove each of the two screws securing the pump head to the pump motor using the supplied 5 mm Allen wrench Support the pump head with your other hand after loosening the two screws moderate force is required Alternative Dismounting Procedure 1 Open the purge valve by turning the black knob on the Pressure Module counterclockwise 2 Switch off the 333 or 334 Pump s
132. o condition the column c Operate the four contact outputs Procedure Switch on the Model 333 Pump after initialization you see the ready to run screen Screen 1 You will see the following soft keys at one time or another Pump Edit to access pump operations Detect to access an associated detector Manual to prime and operate manually Run to run the current Method Program file Pause to interrupt the Method Program Resume to restart a paused Method Program End to stop a Method Program Stop to stop pumping Zero to zero the detector signal if associated Press Manual at the Manual Control screen Screen 8 you will see following soft keys Flow to pump solvents at a specific flow rate Prime to prime specific channels Output to operate the four contact outputs Hydraulic Priming Hydraulic priming is an essential precursor to operating the pump Refer to Page 4 4 for essential information You can prime any actively associated pump 333 334 or 30X from the 333 Master Pump Press Prime you see the Prime screen Screen 25 for each channel the available soft keys are Software Start to start pumping Stop to stop pumping Valve to select solvent valve block channel if fitted Priming Channels Screen 25 shows all of the currently configured channels up to 4 A B C and Sample in this example 1 Open the purge valve to the drain vessel 2 Press the Start soft key correspond
133. o to each pair of twins so that they act in unison The twinned pumps must have the same configuration as their master pumps OO Installation Hydraulic Connections Solvent Inlet Lines For each solvent pump the standard accessory package contains an inlet line fitted with a 20 pm inlet filter Air entering the hydraulic circuit would adversely affect the flow rate Make sure that all connectors are correctly seated and properly tightened SUuO I D9UUOD JIjNepAH i Solvent Inlet Line Proceed with care as follows 1 Remove the plastic plug from the inlet of each Ferrule Gonnecior head 2 Check that the reverse ferrule is correctly seated at the end of the tubing 3 Connect line A to inlet tee piece of Pump A line B to inlet tee piece of Pump B etc When screwing or unscrewing the white connector simultaneously push the tubing so that the end of the tubing touches the bottom of the female port and so that the ferrule is not gripped by the connector which would other wise cause the tubing to twist SOVEN Ia 4 Check that the connectors are tight enough to prevent air from entering the hydraulic circuit 5 In normal use the pump operates with the door closed the solvent line must therefore be threaded through the port to the exterior before placing the inlet filter in the appropriate solvent bottle 6 Clip the solvent lines to the tray Fissure First each tubing is atta
134. oaaiars 4 18 MOM O Or T 4 19 Output e e E sor re ON Cre 4 20 Entering Method Programs sssssesssssssssesssessssstesttserrseenerenessness 4 21 Getting Sitter ssn issu ae een inc Gea 4 21 Creating and Editing Method Programs sesssesseeoes 4 22 Method Program Work Sheet tine wsles eerie 4 29 Pike MaMa CHIE cc cossseeccssesscssae svssesestses sunessasesessossesasssoxsesease asenes 4 30 Procedure aree actuate AA E A a nae 4 30 Good Laboratory Practice GLP Functions 4 33 Procedure kee enters ers eee eects 4 33 UIC PAU eossctsressessecssesusesnaa aetesseneaes sess cressenseesrersceseees ses 4 34 Dismounting Pump Heads and Accessing Maintenance LORS a ccarcecerteerer earners 4 34 Deal installations eee settee eee 4 36 Teak Testo ieee e sets steese E 4 38 Mixing Test e eee e A vmeeeseanr neers 4 38 Running a Method Program sssssssssssssssessssssesstnsstseersrentrsneesness 4 39 Preparing tora Run meee e 4 39 Starting and Stopping a Run cc eecccsenscssccoysseensssssevsgsnssserss 4 39 Post I UnsliMtormnaliOh ee oer ea yee 4 41 JENKO ACIN UEETNEREE 2000500000070000007098000000000060000000000000000000005600000 4 42 Control of A Model 15X Detector s susssssssssesstrstrstrssrrsnrssrssssss 4 44 Miodu E E e 4 44 PORE CHINE e A A arses emarer es 4 44 EAEE IETA OTA sae a cnn aie eens 4 45 PC Software for 333 and 334 Pump Control sceeseeeeee 4 46 5 Maintenance and Troubleshooting Pump bread Maintenance cron icc ccs cscs
135. ommands for 333 and 334 Pumps 7 26 Command Type Description e Run in maintenance sequence status Response format a Where a P during priming phase of the sequence a E when the pump is waiting before to begin the pressurization phase see buffered b command a R during pressurization phase a if no Run In sequence Direct setting of motor frame control This command is for Gilson use only Update current frame This command is for Gilson use only Control the motor rotation This command is for Gilson use only Motor status Response format abcd Where a Rif right motor is running else S b E if right motor error else N c R if left motor is running else S d E if left motor error else N World Wide Web wwwgilson com E mail sales gilson com service gilson com training gilson com World Headquarters Gilson Inc 3000 W Beltline Hwy P O Box 620027 Middleton WI 53562 0027 USA Telephone 1 800 445 7661 or 1 608 836 1551 Fax 1 608 831 4451 Gilson S A 19 avenue des Entrepreneurs B P 45 95400 Villiers le Bel France Telephone 33 1 34 29 50 00 Fax 33 1 34 29 50 80
136. on processes you can create and run Method Programs Bulwild Software Configuring Configuring Introduction To configure you enter descriptions of your pumping system s hardware You verify and where necessary change the configuration refer to Hardware Configuration and Hydraulic Configuration for detailed information As a minimum you must correctly describe and identify GSIOC all pumps the controlling pump Master and those it controls Slaves Additionally you may configure the input output signal parameters safety functions and fine tune the hydraulic parameters refill time inlet pressure compressibility etc Procedure Switch on the 333 Pump then after initialization you see the ready to run screen Screen 1 You will see the following soft keys at one time or another Pump Edit to access pump operations Detect to access an associated detector Manual to prime and operate manually Run to run the current Method Program file Pause to interrupt the Method Program Resume to restart a paused Method Program End to stop a Method Program Stop to stop pumping and Method Program if running Zero to zero the detector signal if associated Software 1 Press Pump Edit you see the Pump Control screen Screen 2 you will see the following soft keys at one time or another File to access the file management operations Edit Create or View to modify an exis
137. onse Complete N 090 01d PUBWIWIOD e eIPEWU 7 7 Introduction to GSIOC Commands GSIOC T Introduction to GSIOC Commands This document includes GSIOC commands for 333 and 334 Pumps are commands for pumps that may detailed in the following tables with their type not be commercially available buffered or immediate and function The response format is described for immediate commands type T For buffered commands type B the parameters are documented There are two devices types input devices and output devices For a 333 Pump input devices are the keypad the contact inputs and the pressure transducer The 333 Pump output devices are the PPMM the contact outputs the display unit screen and the 4 way valve block optional The pump peripheral devices can be either driven by the internal software or by the GSIOC bus A type of software switch actually a dedicated GSIOC command is used to disconnect and reconnect each device from the internal software as illustrated below GSIOC W Bus Input Internal Output device Software device 1 When using any command take care to use the correct command specific syntax A syntax error could have unforeseen consequences 2 The commands and parameters described in this document are case specific You must take care to use the specified case upper or lower GSIOC Commands for 333 and 334 Pumps Operational Functions
138. outlet check valves piston assemblies Quality References Individual Quality Control Report Flow Rate Accuracy and Repeatability Conditions Automated gravimetry water 20 23 CC 988 1038 hPa 45 75 humidity 0 9968 g ml 5 ml min 10 2 MPa default values for all adjustment parameters Six measurements of 1 minute each after a less than 30 minute run with a new piston seal Limits of Acceptance Accuracy bias lt 1 Repeatability SD lt 0 3 lt 0 2 after a more than 30 minute run with a new piston seal Operational Qualification Procedure Leak Test Duration Approximately 10 min Conditions Pressure 15 MPa Limit of Acceptance Pressure decay lt 10 in 5 min Complete Procedure for Composition and Flow rate Duration Less than 2 hours in total Conditions Solvent A is methanol solvent B is methanol plus 0 3 acetone 10 ml min 1 2 MPa mixing test program pre stored under GLP Mix to be recorded as file 20 Three cycles of 27 5 min each including composition ramp and steps UV absorbance measurement 265 nm 500 mAUFS One measurement per step Digital flowmeter typically 1 l min resolution 0 2 0 3 ml priming volume A accuracy bias R repeatability RSD Six measurements Le eed jed1UYyoeL Technical Data Reference Information Limits of Acceptance Flow rate accuracy bias lt A 2 Flow rate repeatability RSD lt R 0 77 Composit
139. oy Screen 1 Pump file 19 000 ml min Screen 2 Pump control 19 Screen 82 Audit trail Maintenance logs Seal installation eak tes Qualification tests Audit Maint Seal Leak Qualif 4 33 Software Good Laboratory Practice Functions 4 34 Audit Trail Starting from the GLP Screen 82 press Audit Screen 83 then use the arrow keys to move the cursor to the field you wish to change To switch on or off the audit trail select the Audit trail used field press Change to select ON or OFF then press ENTER Date and Time 1 Select the Date field key in the date as a 6 digit number ddmmyy for example 140299 then press ENTER 2 Select the Time field key in the time as 4 digits separated by a point hours minutes for example 22 35 then press ENTER The date and time are retained when you switch off the 333 Pump or in the event of a power failure 3 Press ESC to return to Screen 82 Dismounting Pump Heads and Accessing Maintenance Logs This series of screens enables you to review and if required after changing a pump head reset the maintenance logs for each of the currently configured 333 and 334 pump heads In addition the dismount procedure is required in order to be able to change a piston seal or a piston assembly Starting from the GLP Screen 82 press Maint to access Maintenance logs Screen 84 you will see these soft keys at one time or
140. p 40 R W Link application 1 to 24 41 R W Number of loops 1 to 999 N sduind peg pue ggg 10 spuewwog 7 13 GSIOC Commands for 333 and 334 Pumps 7 14 Command Type Description Code Type Parameter Units Range 42 R W L Restart after power failed option 0 means Stop 1 means Continue current application 2 means Start power failed application 43 R W Application locked 0 if application unlocked not equal 0 if application locked 44 R W L Pump C head size code 33X 200 for 333 334 can t be changed if pumping 45 R W L Reserved for 32X 46 R W L Pump C inlet pressure 1 10 MPa 0 to 500 47 R W L Reserved for 32X 1 10 MPay 0 to 500 48 R W L Reserved for 32X ms 125 to 1000 49 R W L Reserved for 32X ms 125 to 1000 50 R W L Pump C Liquid compressibility Mbar 0 to 2000 used in HPM mode only 51 R W L Reserved for 32X Mbar 0 to 2000 52 R W L Inj pump head size code 30X 5 10 25 50 can t be changed if pumping 100 or 200 53 R W L Inj pump Inlet pressure 1 10 MPa 0 to 500 54 R W L Inj pump Refill time ms 125 to 1000 55 R W L Inj pump Liquid compressibility Mbar 0 to 2000 56 R W L High pressure limit 1 10 MPa 0 to 600 for 333 334 must be higher than low pressure limit 0 to 300 for 331 332 57 R W L Low pressure limit 1 10 MPa 0 to 600 for 333 334 must be lower than high pressure limit 0 to 300 for 331 332 5
141. p bottle tray 1 E66231 Bellows mounting tool POM white piston assembly for pump heads 1 Electrical 500933 GSIOC cable 1 500006 Power cord 110 V 1 500005 Power cord 220 V 1 Documents Reference Description Quantity 804035 Quality control certificate 333 and 334 Pumps 1 None Quality control report 333 and 334 Pumps 1 801397 Unpacking notice 1 Reference Information Additional Accessories for 333 and 334 Pumps Reference Description Hydraulic E66250 Gilson 864 degasser 4 channel PTFE and PPS 9 2 ml 70 hPa 400141 Piston seal PTFE black flange type Hastelloy C276 spring for H3 pump head E66387 Four solvent selection valve block PTFE fully equipped for 333 and 334 Pumps includes 1 x 866383 Valve block 4 solvent without holder and tubing for 333 and 334 Pumps 1 x E66369 Holder valve block for 333 and 334 Pumps 3 x E66381 Tubing FEP 3 2 x 4 8 x 1250 mm for 333 and 334 Pumps 1 x E66370 Tubing FEP 3 2 x 4 8 x 150 mm with fittings from valve to tee piece 1 x E66375 Tee piece PTFE 5 16 24 TPI for 3 16 tubing 3 x E66158 Tubing clip for bottle tray 4 8 mm 3 16 333 and 334 Pumps clips tubing to tray E66464 Fraction collection valve block PTFE fully equipped 33X Pumps includes 1 x 866053 Valve block 4 solvent without holder and tubing 32X Pumps 1 x E66124 Holder valve block 32X and 33X Pumps 1 x 420564 Tubing FEP 1 6 x 3 1 x 4000 m
142. pecial tubing ref E66360 from the Tee piece of the Slave Pump to the inlet on the 333 s PPMM prime the system refer to Chapter 4 3 21 Installation 3 Setting up 3 22 Configuration Example 2 Solvent Mixing and Injection A 333 Pump may be set up to control the flow and composition on a time variant gradient or a time invariant isocratic basis to carry out sample injection a 30X Pump must also be associated with the 333 Pump In this case the 333 Pump controls the injection pump flow and composition Solvent B is routed via a Tee piece to an inlet on the PPMM of the Master 333 Pump where the two solvents are combined at high pressure Setting up What You Must Do 1 Switch on the pump s check and set their GSIOC IDs the start up screen appears briefly Screen 0 then make the electrical connections between the instruments 2 Check and if necessary change the software configuration at the Run Screen 1 press Edit or Pump if linked to a Gilson 15X Detector at the Pump Control Screen 2 press Config for anew pump the Configuration Screen 50 shows 333 as the model H3 as the head type he Injection from pump NO Maximum number Un eT I of solvents ONE eee ATOKA 0 8 to add solvent pump B press Hard Screen 78 appears at Extra solvent id 2 press Change until you see 334 or 333 press ENTER to add the injection pump press the down arro
143. ping 50 for H2 200 for H3 15 R W L Piston mode can t be changed if pumping 2 for DUAL piston mode 16 R W L Pump A Inlet pressure 1 10 MPay 0 to 500 17 R W L Pump B Inlet pressure 1 10 MPa 0 to 500 18 R W L Reserved for 32X Pumps ms 125 to 1000 19 R W L Reserved for 32X Pumps ms 125 to 1000 20 R W L Reserved for 32X Pumps Mbar 0 to 2000 21 R WL Reserved for 32X Pumps Mbar 0 to 2000 22 RL Nb of solvents 1to3 can t be changed if pumping 23 R W L Mixing mode 0 for HPM can t be changed if pumping 24 R W L Injection mode 0 for no injection can t be changed if pumping 1 for injection 25 R W L Signal output profile 0 for PRESSURE 1 for FLOW 2 for of pump A 3 for of pump B 4 for of pump C 26 R W L Delay volume for signal 1 10 ul O to 900000 output profile 27 R W L Contact output pulse duration 1 100 min 1 to 100 28 R W L Audit trail option 0 if ON 1 if OFF 29 R W L Contact input PAUSE 0 if Pause with without flow without FLOW 1 if Pause with FLOW 30 R W L Elution pump synchronization 0 if synchronization before injection OFF 31 R W L Reserved parameter Gilson only 32 R Pause time 1 100 min 0 to 999999 33 R Wait contact time 1 100 min 0 to 999999 34 R W Date time min 0 to 23 x 60 59 35 R W Date day 1 to 31 36 R W Date month 1 to 12 37 R W Date Year 0 to 99 38 RL Pump model 3 for 33X 39 RL Remote pump 0 for Master Pump 1 for Slave Pum
144. r 92 Alternatively provided the first step 1 is completed correctly you may press Scan to identify any connected pumps which are then added to Screen 78 next to their currently configured IDs You are now ready to create your Method Program file s Optionally you can modify advanced configuration features refer to Chapter 4 3 Make the following hydraulic connections from the Outlet Filter of the Master 333 Pump to the downstream Tee piece solvent line A to the inlet Tee piece on the Master 333 Pump solvent line B to the inlet Tee piece on the Slave 334 Pump special connector ref E66360 from the outlet Tee piece of the Slave Pump to the inlet of the 333 s PPMM prime the system Chapter 4 OF Outlet Tee piece Outlet Tee 30X Pump Heads fy Inlet Tee PPMM 1 Pump ID 4 Sample f I Solvent A Pump ID 1 oO dn bulyeas Outlet Heads Inlet Tee Solvent B Pump ID 2 or3 3 23 Installation 3 Configuration Example 3 333 334 Pumping System with Control from a PC Setting up The 333 Pump Solvent A at the left is fitted with a PPMM To connect to t
145. ramic piston UHMWPE standard piston seal ruby check valve ball sapphire check valve seat and titanium body Maximum pressure 21 MPa Stroke volume 1595 ul Minimum piston cycle time at 200 ml min 956 ms for atmospheric pressure 881 ms for 21 MPa 1500 Mbar 1 each piston delivering during half of the cycle Maximum instantaneous inlet flow rate 399 ml min during 227 ms Dead volume 848 yl Piston rinsing chamber volumes 4 0 ml total and 1 2 ml stroke 75 ml min for 200 ml min solvent delivery Pressure Purge and Mixing Module PPMM Identification Gilson 866344 plus serial number Flow path materials 316 steel body pressure transducer grid and packing balls PEEK mobile seal and PTFE fixed seal Internal volume 2 85 ml 0 1 ml 15 2 mm ID cylinder packed with forty one 5 mm balls Maximum pressure 30 MPa Number of ports six 2 1 mm diameter external through holes Outlet Filter Assembly Identification Gilson 410707 Upchurch S 1579 Flow path materials 316 steel body and frit filter ETFE frit ring Internal volume 160 pl 2 1 mm diameter through holes Filter 10 pm 1 6 mm thickness 19 mm diameter Gilson 410730 Upchurch A331 6 9 Reference Information Technical Data High pressure Plumbing Filter 316 steel 10 pm 19 mm diameter 1 6 mm thickness 81 pl for 3 2 mm 1 8 tubing Tubing upstream from the filter 316 steel 2 1 x 3 2 mm 1 8
146. ransmitted If the pump received several commands at the same time or in the mean time it is not possible to know where the error is T l Read Audit Trail file line Returns event pointed by Audit Trail line pointer Response format Event code YY MM DD HH mm par1 par2 where Event code is the event code see below YY is the year 0 to 99 MM is the month 1 to 12 DD is the day 1 to 31 HH is the hour 0 to 23 mm is the minute 0 to 59 Par1 is the first additional value 0 to 255 Par2 is the second additional value 0 to 65535 Some parameters are not required for all events In this case the parameter exists in the response but has no meaning When the pump data base is busy the response is so try again If there are no available events or if the audit trail line pointer reaches the last line the response is This command increments automatically the Audit Trail line pointer Use immediate T command to set pointer at the beginning of the file GSIOC Command Type Description continued Event Code Event Designation Par1 Par2 a Start of application Application number b End of application c Stop application d Pause application e Resume application f Application modification Application number g Configuration modification h Pressure limit reached 0 for high pressure limit Pressure limit in tenths of MPa i Counter change
147. rate and composition that existed when that soft key was pressed A pause time counter replaces the run time counter until you press End or Resume Pressing Resume restarts the Method Program from the point at which it interrupted Pressing Stop during a pause stops pumping until you press Resume Whenever you press End the Method Program is terminated but pumping continues at the rate and composition that existed when that soft key was pressed After pressing Stop you may need to press End to terminate the Method Program When a Method Program comes to an end the pump continues to pump at the flow rate and composition that were applicable at the last programmed event or at the end of n loops unless you program a flow rate of zero at the end of the program or link the run file to a stop program otherwise you must press Stop to stop pumping You can press the Edit key to access and change the Method Program parameters even when the Method Program to be edited is running When you see the word running after the file number on selected screens it means that the Method Program is either running or paused it does not refer to the pistons which may be pumping or stopped Likewise the absence of the word running does not imply that the pistons are not in motion Software Post Run Information At the Pump control screen Screen 2 press Watch to obtain the following post run information the mi
148. re physical properties compiled from the Handbook of Chemistry and Physics 79 edition D R Lide CRC Press 1998 1999 F_and AP L are examples of basic hydrodynamic calculations P is the polarity calculated by L R Snyder Journal of Chromatographic Sciences 16 223 1978 from experimental measurements by L Rohrschneider Analytical Chemistry 45 1241 1973 oO fav oO 5 2 3 z 2 Y 2 v 5 5 5 o S S 5 D Q x K S D z O D lt D T A UVC nm 180 205 190 212 205 195 233 RI 1 333 1 329 1 344 1 406 1 378 1 376 1 424 BP C 100 65 82 66 82 69 40 VP hPa 32 169 118 216 60 202 582 n cP mPa s 1 00 0 60 0 37 0 55 2 3 0 33 0 44 p g ml 0 997 0 79 0 78 0 88 0 78 0 66 1 32 n p cP g mi 1 00 0 76 0 47 0 62 2 9 0 50 0 33 X Mbar 46 123 99 93 100 160 97 F ml min 28 21 13 18 83 14 9 4 AP L MPa m 0 17 0 10 0 06 0 10 0 40 0 06 0 08 P 10 2 5 1 5 8 4 0 3 9 0 1 3 1 UVC UV cutoff RI refractive index at 20 C BP boiling point at 1013 hPa VP vapor pressure at 25 C n kinematic viscosity at 20 C p density at 20 23 C F critical flow rate for a 0 25 mm ID tubing F ml min 113 x 0 25 mm x n cP p g ml AP L linear pressure drop for 1 ml min and 0 25 mm ID tubing AP L MPa m 6 8 x 10 x 1 ml min x 100 cm x n cP 0 25 mm X compressibility at 20 C Reference Information Safety Data for Flammable Solvents For
149. ring by 5 mm undo the terminal s fixing screw push the bared wire into the corresponding hole in the terminal block and then tighten the fixing screw using a small screwdriver Pressure Flow A B C D Digital Output 0 1000 mV Analog Output 142 1000 mV oO SUOIJEDIUNWIWOYD SUOI DOUUOD e911 99 9 3 3 Installation Electrical Connections Communications 14 pin Connector Output 1 Output 2 Output 3 Power Contact Output 4 12 V 500 mA 0 Volt DC Output 12 V Relay Coil Powering an External Relay A 12 V 500 mA DC supply is available at the right most pair of pins of the left hand terminal This supply can be switched manually from the control panel or automatically from a Method Program by connecting it to one of its neighboring outputs Output Signals a Four two way relay type outputs are available via the left hand socket Each of these outputs is electrically isolated from the others and from ground Switching from the normally closed to the normally open position takes place under software control see Chapter 4 at pre programmed times You can program these contacts to Open Close or Pulse for a specific duration You connect one wire from the receiving device to the common terminal of Output 1 2 3 or 4 and a second wire to either the corresponding normally open or normally closed terminal depending on th
150. s ANGIVE 2000006920900000 00000 6 14 Principle a e 6 14 Adjustments e e E EEE 6 15 Properties of Common Solvents 47 s eccceqe ences 6 16 Safety Data for Flammable Solvents sass sees 6 17 DEAT OI E E E E 6 17 NIRE E e E A ee ns 6 18 Abbreviations for Thermoplastic Materials 6 19 Part NUMBERS aee e 6 20 Gilson 399 PUMP e e 6 20 Gilson SIH PUMP eee idan eaas 6 22 Additional Accessories for 333 and 334 Pumps 6 23 7 GSIOC Physical bevels crcciuectecaas rata cacauntaeus 7 2 G5lOC Control Cable m 7 2 GSIOC Connector Pin Functions s cee ce ccsersecscsssssseresirese 7 2 Peet cele ey eles tee cna centers atten tees ae eee 7 3 Bit Rates ee oreo se ee ee cera eeee 7 3 GSIOC IDS e e e ee e e 7 4 haracter devellSe IONE 2200000500000500090000209900000000000000000000900000000 7 5 Disconnect and Connect Sequences ese 7 6 Immediate Command Protocol eee e ae en 7 7 Introduction to GSIOC Commands sas ceen aes 7 8 Commands for 333 and 334 Pumps assscccsarscsseesenssevse cseesseeesas 7 9 Oane PunchOns acs son cree ee cae 7 9 Mamen e UNC ONS ee erect e teeter nee 7 10 Description ct Commands ee vesce scaeccs ster cee 7 10 Table of Contents 4 Safety Read this section carefully before installing and operating the pump For safe and correct use of the pump it is essential that both operating and service personnel follow generally accepted safety procedures as well as the safety instructions given in this document the
151. s ENTER For a 334 Pump the bit rate 9600 19200 or External is set mechanically using the right hand of the two selectors on the rear panel GSIOC Electrical Level GSIOC IDs The GSIOC IDs may be changed where the pump s are being controlled from a computer In which case the configured IDs must correspond to those set using the controlling software For each level i e from one Master the GSIOC identification number ID that you set must be unique for each item of Gilson equipment For a 333 Pump the ID 0 63 is configured as follows 1 Switch on the pump wait until initialized 2 Press in turn Edit Config Misc 3 Key in the desired ID for the 333 Pump then press ENTER For a 334 Pump the ID 0 9 is set mechanically using the left hand of the two selectors on the rear panel GSIOC Character Level and Format Because the GSIOC is a multi drop channel with the ability to have several slave units connected at the same time GSIOC reserves some of the possible characters for channel control The data format is asynchronous serial with one start bit eight data bits one even parity bit and one stop bit Any parity error can be corrected by reconnecting and restarting the message w r Function aD NOAR ON O0OO0 start bit value 1 value 2 value 4 value 8 value 16 value 32 value 64 address flag if high parity even stop optional Or the last character
152. s own name remains disconnected 5 After the slave device is connected the master device may send a command immediate or buffered as described in the following Sections The selected device remains active until it receives the disconnect code FF hexadecimal or the binary name of a different slave device GSIOC Immediate Command Protocol Immediate commands which are always in the form of a single character request status reports from a slave device for example what kind of device are you what is your current operating mode what are you doing now When a master device issues an immediate command to a designated slave the slave Start interrupts its current job to respond to the immediate high priority command sng Immediate After a slave device receives an immediate Command command it answers the request with the first character of its response The master checks the value of the ASCII character If the character s value is less than 128 it responds to the slave with an ACK character 06 hexa decimal This exchange continues until the slave sends the last character of the response Send ACK To indicate that the last character is being sent the slave adds 128 10000000 binary to the characters value 20 ms Timeout Error Handler In response to an unrecognized immediate command a slave responds with the pound sign Immediate Resp
153. second 333 Pump Solvent B is routed via the outlet Tee piece of the 334 Pump to an inlet on the PPMM of the Master 333 Pump where the two solvents are combined at high pressure When three solvents are to be combined a second slave pump can be connected to the PPMM Setting up What You Must Do 1 Switch on the pump s check and set their GSIOC IDs the start up screen appears briefly Screen 0 then make the electrical connections between the instruments including the GSIOC cable linking Master to Slave OO dn 6ulnes Installation 3 Screen 1 Pump file 000 ml min O A Setting up Screen 2 Screen 50 Configuration Configuration Model 333 Model 333 Injection from pump NO Injection from pump NO Controlled pump 33X 2 Maximum number of solvents ONE Maximum number of solvents TWO Screen 78 Model 333 Hardware Configuration Controlled pumps for Hardware Configuration del 333 ontrolled pumps for Extra solvent id2 None Extra solvent id3 None siue Someni NY ere tiron e EE id4 None oe In the Figures given in this Chapter The key to push is 2 Check and if necessary change the software indicated by the lighter color configuration soft key follow the path at the Run Screen 1 press Edit or Pump if indicated by the arrows When linked to a Gilson 15X Detector aac ae at the Pump Control Screen 2 press Config sie iniented a bold
154. see above To define an application first send the editing application number add events see G and H commands and then send all parameters defining this application the parameters have to be consistent Code Type Parameter Units Range 78 80 81 82 83 84 85 86 87 88 89 90 to 79 R W L R W L R W L R W L R W L R W L R WL R W L R W L R W L R W L Reserved Pump A selector A1 Solvent Compressibility K Pump A selector A2 Solvent Compressibility K used only if solvent selector is fitted to Pump A Pump A selector A3 Solvent Compressibility K used only if solvent selector is fitted to Pump A Pump A selector A4 Solvent Compressibility K used only if solvent selector is fitted to Pump A Pump B selector B1 Solvent Compressibility K Pump B selector B2 Solvent Compressibility K used only if solvent selector is fitted to Pump B Pump B selector B3 Solvent Compressibility K used only if solvent selector is fitted to Pump B Pump B selector B4 Solvent Compressibility K used only if solvent selector is fitted to Pump B Pump C selector C1 Solvent Compressibility K Pump C selector C2 Solvent Compressibility K used only if solvent selector is fitted to Pump C Pump C selector C3 Solvent Compressibility K used only if solvent selector is fitted to Pump C Mbar Mbar Mbar Mbar Mbar Mbar Mbar Mbar
155. selected display line The selection of the line is done using the buffered W command The characters returned are the real contents of the physical display not the message produced by the internal software Comment The first line to be returned is the last entered by the buffer W write command If the write command has not been used the upper line is read at the first occurrence of the read command the second line is read at the second and so on Read display buffer Response format as for immediate W command Comment reading mechanism same as immediate W command The response is the image of the display line if it were connected to the internal software This is also the message which will be restored to the display after a reconnect command GSIOC Command Type Description Z Read compression stroke Response format aaaa bbbb Where aaaa is the Head A compressibility stroke if flow gt zero in one thousandth of the actual piston stroke 0 to 1000 bbbb is equal to 0 and has no meaning in this context Actual Stroke Complete Stroke multiplied by of stroke Dismount Mount heads Syntax an Where n D means send the two pump heads to the dismount position both heads simultaneously n N means to initiate the head mounting sequence both heads simultaneously Start maintenance sequence Syntax bnm p q Where n 0 gt Start lt To run in new pisto
156. signs a value to a parameter Syntax Ennn mmmmmmm where nnn is the parameter code see below mmmmmizm is the value assigned to the parameter The following list identifies the code assigned to each parameter it also gives the range of values that can be entered For type R W Read Write R Read only L available for N command Code Type Parameter Units Range 0 R W Application number selected to run RFile 1 to 24 1 R W Application number selected for edition EFile 1 to 24 2 R Currently running application number CFile 1 to 24 3 R Application state returns 0 if STOP 1 if RUNNING 2 if PAUSE 3 if WAITING CONTACT 4 if WAITING CONTACT and PAUSE 5 if INJECTING 6 if INJECTING and PAUSE 4 R Running Elapsed time 1 100 min 1 to 999999 5 R Total flow rate of the pumping system 1 10 ul min Per pump 0 to 50000 for H2 Per Pump 0 to 2x10 for H3 GSIOC Command Type Description Code Type Parameter Units Range 6 R Percentage of Solvent A 1 10 0 to 1000 7 R Percentage of Solvent B 1 10 0 to 1000 8 R Percentage of Solvent C 1 10 0 to 1000 10 R Reserved for the SF pump 11 R W Pressure unit 0 for MPa 1 for bar 2 for psi 12 R W Alarm 0 if beeper on alarm is OFF 1 if beeper on alarm is ON 13 R WL Pump A head size code 50 for H2 can t be changed if pumping 200 for H3 14 R WL Pump B head size code 50 for H2 can t be changed if pum
157. t the fully withdrawn position in fact if you turn the retaining screw fully counterclockwise you reach another stop and risk unscrewing the mechanism at the fully out position if excessive force is used O1 aoueudjUIeWy peH dung Maintenance and Troubleshooting e Pump Head Maintenance White Cap Piston and Bellows Rinsing Chamber Pumping Chamber Piston Seal a Replacing a Piston Seal The following steps should be carried out on a clean dry surface No special tools are required 1 Pull apart the two halves of the pump head with a slight twisting motion 2 Remove the piston seal either by a carefully levering out the seal using the end of the Allen wrench in which case the seal must be discarded or b blocking the outlet and using an air line inserted into the center of the seal to blow the seal out of the recess in the pump head 3 Clean out any debris from the old seal remaining in the recess using a soft cloth or an air line 4 Push a new seal carefully into the recess Only use the type of seal specified in Chapter 6 5 Initialize and run in the new seal s Piston Rinsing Chamber When a pump is delivered the inlet and outlet ports to the rinsing chamber are fitted with plugs which prevent airborne particles from entering the ports If you do not need to use piston rinsing you should leave these plugs in place If you pump a liquid containing more than 0
158. t type see below 4 23 Software Entering Method Programs 4 24 After keying in one of a series of parameter values pressing ENTER automatically moves the cursor on to the next parameter However you may use the horizontal arrow keys lt 4 gt to move the cursor to the parameter that you wish to modify Creating a New File Screen 30 Screen 39 Screen 36 Screen 36a Screen 36 HF Hie Select x 3 Press Confirm then Add to add an event of the same type returns to Screen 36 or Select to choose a different event type returns to Screen 39 4 Continue to cycle between Screens 36 and 36a Add or Screens 36 36a and 39 Select until you have completed the schedule of events Normally you would enter the complete profile for events of one type before using Select to access the next parameter type e g FLOW then COMP followed by INJ WAIT and OUTPUT If the events are not entered sequentially the software automatically sorts them into the correct time order 5 When done press ESC to return to Screen 30 Here by pressing Consump you may access solvent consumption per loop for the currently configured channels Screen 32 press ESC to return to Screen 30 Editing an Old File Screen 30 Screen 35 Screen 36 Screen 36a Screen 36 A Software FLOW 1 Key in a time 0 00 to 9999 minutes then press ENTER 2 Key in a flow rate 0 to 400 ml min
159. ted Archive the audit trail PC then reset the audit trail Validation process has restored default parameter s Check all Method Program and configuration parameters RAM error contact your Gilson representative Contact your distributor Maintenance and Troubleshooting Electrical amp Program Problems Problem Possible Causes Solutions Pump does not operate no POWER indicator LED No power or fuse blown Check fuses plug in power cord switch on at rear Pump does not operate no ON indicator LED Pump is not operational Press the ON OFF key on the standby panel Pump does not stop at the end of a run Not programmed Program a flow rate of zero and a composition of zero at the desired end time for all solvents Error LED lights up Various See text Slave pump does not operate No GSIOC communication Check GSIOC cable s are connected correctly between pumps and that GSIOC ID s are correctly set Pump X is missing message appears on the screen No GSIOC communication or the Slave Pump X is not switched on Switch on the Slave Pump check GSIOC connectors the baud rate and ID of the slave O1 BuljooysajqnoiL Maintenance and Troubleshooting Troubleshooting Hydraulic Problems Problem Possible Causes Solutions Air bubbles in both the inlet and
160. ting Method Program file Create Edit or View to enter a new Method Program file View Edit or Create to read only an existing Method Program file Config to enter configuration parameters GLP to access audit maintenance run in and test functions for a 333 pump Watch to obtain post run information 2 Press Config you see the Configuration screen Screen 50 which indicates the model and head type for the Master pump and any pumps under its control Inside this mainly descriptive screen you can activate an associated sample injection pump The available soft keys are Safety to access high and low pressure limits restart and malfunction options I O to access specific Input Output functions pulse length output signal type etc Misc for GSIOC id bit rate units display contrast screen saver beeper ON OFF Hard to change the pump model and identify any controlled pumps Hyd to access hydraulic parameters such as Inlet Pressure and Compressibility When setting up a new system you should proceed by reviewing and changing where necessary these items in the following order Hard Hyd Safety I O and Misc Screen 1 Pump file 000 ml min 0 0 A_ 0 0 B Screen 2 Screen 50 Configuration Model 333 H3 Injection from pump NO Maximum number of solvents ONE Safety Change Hard 1 The top line of the in run screen is reserved for a Model 15X detector if associat
161. uire a special shaped tubing E66360 In order to maximize the available as a standard accessory Solvent B is routed a pala a j umping System it is important via the outlet tee piece of 334 Pump to an inlet on that you use only the special the PPMM of the 333 Pump where the two solvents shaped tubing to link the two are mixed at high pressure pumps The tubing linking the two pumps goes through the tubing port together with solvent and rinsing port tubings In the figures the tubing port is in the position where the tubings are locked in place To make it easy to install and to remove tubings there is a fissure in the tubing port which is accessed by rotating the tubing port until the fissure lines up with the opening in its housing Ma Connecting Tubing Side by side Configuration Ref E66360 f Sa Y Tubing Port oO sduing 9y HBuluol isog Installation Positioning the Pumps 3 16 Connecting Tubing 1 j Vertical Stacking L Ref E66451 In order to maximize the performance of your 333 334 Pumping System it is important that you use only the special shaped tubing to link the two pumps Vertical Stacking Where bench space is at a premium the pumps may be stacked one on top of the other The 333 Pump Solvent A at the top is fitted with PPMM and outlet filter To connect to the 334 Pump at the bottom you require a special shaped tubing E66451 available as an additio
162. uld also switch off the power using the main ON OFF switch on the back panel of the 333 or 334 Pump s u uodwo 01 U04D dwnd SEE 2 7 Rear Panel Electrical Connectors Description 2 Rear Panel Electrical Connectors All electrical connections are made to the rear panel Also visible are the fan s ventilation slots which must never be obstructed in any way The function of each item is as follows 1 Main power ON OFF switch 2 Power supply cable socket 3 Fuses and voltage selector 4 14 pin connector socket for output contact signals relay type 5 10 pin connector socket 4 input signal channels and 2 output channels 1 digital output converted to analog pin 9 0 1 V configurable 1 analog output pin 10 142 1000 mV for pressure 6 GSIOC from controller 333 Pump or computer 7 GSIOC to slave pump 333 334 Pump and or 30X Pump or Gilson 15X UV Detector 14 pin Connector GSIOC Connectors 10 pin Connector Solvent Tray Ventilation Slots SHANNA e N Rear Panel Fixing Screw 1 of 4 RELEEOLELES ON OFF Switch Ventilation Slots Description For a 334 Pump which has no other type of connector a pair of rotary switches for setting GSIOC ID number setting and bit rate replaces the left most GSIOC socket Power Connector The standard 3 pin connector accepts the power supply cord supplied with your 333 or 334 Pump Power supply cord reference 500005
163. uted before it ends With reference to Screen 30 if necessary move the cursor using the vertical arrow keys to the Number of loops line key in a number between 1 and 999 then press ENTER Linking Files sweibojg poya Gulse uy You link files so that they will be executed as a chain that is they will be run one after the other starting with the file currently selected With reference to Screen 30 if necessary move the cursor using the vertical arrow keys to the link to file line press the Link to key in the number of the file 1 24 to which the current file is to be linked and then press ENTER To undo a link you must press the No Link key Listing Events At Screens 36 or 36a press List to list all of the events entered in the currently selected file the possible soft keys are Delete to remove an event from a file Time Flow to toggle between injection flow rate and duration Change to change the state of an output Select to select an event type from Screen 39 As well as reviewing a Method Program file you may change the parameters In either case you use the vertical arrow keys A and W to scroll through the list of events and to move the cursor from one parameter field to another After keying in each new value you must press ENTER to confirm the value and move the cursor on to the next parameter 4 27 Software Entering Method Programs 4 28 Deleting Events
164. w key at Injection id 4 press Change until you see 30X press ENTER File Greate Gontig Watch GLP to enable sample injection press ESC then at configuration Screen 50 press Change select YES press ENTER Screen 50 Configuration Configuration Screen 2 Configuration f Model el 333 Model 333 Injection from pump NO injection from pump Injection from pump NO Controlled pump 33X 2 SOK Controlled pump ey 30X 5 4 Maximum number of solvents TWO Maximum suse of solvents TWO Maximum number of solvents TWO _____ Safety 1 0 Misc Change Hard Hyd Screen 78 Hardware Configuration tah Hardware ee 0 Model 333 Controlled pumps for Kodel pag pumps for rete solvent Extra Solvent id3 Bag solvent i ectio Installation the Configuration Screen 50 should now show 333 as the model H3 or H2 as the head type Injection from pump YES Maximum number of solvents TWO then for each solvent pump if head type does not match those fitted to either pump press Hyd then at the next screen 90 for Solvent A 91 for Solvent B etc select the solvent pump to change by pressing the Next or the Prev key select Head type press Change until you see the head type fitted H3 press ENTER head size and other parameters for the injection pump Screen 94 can be accessed by pressing the Inject soft key at Screen 90 91 o
165. xample errors during the entry of Method Program or configuration parameters For this type of error the software displays messages that explain the required corrective action However there are some critical error situations that can occur during or after a run Message Corrective Action Pressure lower than X Check for leaks check configuration parameters check and possibly rerun Method Program file Pressure higher than Y Check hydraulics check configuration parameters check and possibly rerun Method Program file Input 2 was activated Check hydraulics check configuration parameters check and possibly rerun Method Program file Power restored after failure The latest run could be invalid Check the system before a possible rerun of this file Channel Z failing Failure may be caused by a blockage tubing check valve etc Check the hydraulics especially Channel Z check configuration parameters check and possibly rerun Method Program file Communication fails with N Check that pump N is switched on Check GSIOC ID and connections File does not exist Check that you are trying to run a valid file Check that any linked files are valid Maintenance limit is passed for M Service item M and reset the counter see Chapter 4 Config GLP Audit trail is satura

333 and 334 Pumps User's Guide

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