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Agilent 1200 Series Capillary Pump User Manual

1. 1 Place the support rings on the plunger housing plungers 2 Tighten the lock screw not installed and snap the pump head and plunger housing together Lock screw Pump head Plunger housing 142 1200 Series Capillary Pump User Manual Maintenance 7 Simple Repair Procedures 3 Carefully insert the plungers into the pump head assembly and press them completely into the seals Plunger Pump head assembly l 4 Slide the pump head assembly onto the pump drive Apply a small amount of pump head grease to the pumphead screws and the balls of the spindle drive Tighten screws stepwise with increasing torque Balls of spindle drive Pump head screws AIV connector Inlet tube Active inlet valve i Nl 5 Reconnect the capillaries tubing and the active inlet valve cable to the connector 1200 Series Capillary Pump User Manual 143 7 Maintenance Exchanging the Optional Interface Board When Board defective Parts required Description 1 BCD Interface board see service manual CAUTION Electrostatic discharge at electronic boards and components Electronic boards and components are sensitive to electrostatic discharge ESD gt In order to prevent damage always use an ESD protection for example the ESD wrist strap from the accessory kit when handling electronic boards and components Switch OFF the capillary pump at the main power switch
2. 2 8710 0806 Wrench open end 1 4 5 16 inch Qty 1 8710 0510 Wrench open end 14 mm Qty 1 8710 1924 Wrench open end 4 mn Oty 1 8710 1534 Hex key 2 5 mm Qty 1 8710 2412 Hex key 3 0 mm Qty 1 8710 2411 Torque Adapter G1315 45003 Insertion Tool Oty 1 01018 23702 ESD Wrist Strap Oty 1 9300 1408 Can cable 1 m long 5181 1519 Hex key 4 mm 15 cm long T handle 8710 2392 Solvent inlet filter x4 01018 60025 Purge valve assembly G1311 60009 Purge valve holder G1312 23200 Capillary 550 mm 50 pm G1375 87310 1200 Series Capillary Pump User Manual 155 8 Parts and Materials for Maintenance Capillary Pump Accessory Kit 156 1200 Series Capillary Pump User Manual 1200 Series Capillary Pump User Manual 9 Identifying Cables Cable Overview 158 Analog Cables 160 Remote Cables 163 BCD Cables 168 Auxiliary Cable 170 CAN LAN Cables 171 External Contact Cable 172 RS 232 Cable Kit 173 a Agilent Technologies 157 9 Identifying Cables Cable Overview Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Type Description Part Number Analog cables 3390 2 3 integrators 01040 60101 3394 6 integrators 35900 60750 Agilent 35900A A D converter 35900 60750 General purpose spade lugs 01046 60105 Remote cables 3390 integrator 01046 60203 3392 3 integrators 01046 60206 3394 integrator 01046 60210 3396A Series integrator
3. A2 Second plateau negative or other plateau positive Probable cause 1 Leaking outlet valve in channel B 2 Loose pump head screws in channel B 3 Leaking seal or scratched plunger in channel B2 Suggested actions Clean the outlet valve in channel A Ensure the sieve in the outlet valves are installed correctly Tighten the outlet valve Ensure the pump head screws in channel A are tight Exchange the pump seals in channel A Check the plunger for scratches Exchange if scratched unstable and at least one Suggested actions Clean the outlet valve in channel B Ensure the sieve in the outlet valves are installed correctly Tighten the outlet valve Ensure the pump head screws in channel B are tight Exchange the pump seals in channel B Check the plunger for scratches Exchange if scratched 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics Third plateau negative or unstable and at least one other plateau positive Probable cause 1 Airin channel A or new seals not yet seated 2 Loose active inlet valve in channel A 3 Loose pump head screws in channel A 4 Loose outlet valve in channel A 5 Leaking seal or scratched plunger in channel Al 6 Defective active inlet valve in channel A 1200 Series Capillary Pump User Manual Suggested actions Flush channel A thoroughly with isopropanol under pressure use restriction capillary Tighten the active inlet val
4. Leak sensor not installed Solvent selection valve Figure 1 Overview of the Capillary Pump 1200 Series Capillary Pump User Manual 9 1 10 Introduction to the Capillary Pump Hydraulic Path Overview The capillary pump is based on the Agilent 1200 binary pump and performs all the functions necessary for a u flow solvent delivery system Basically these functions are e Low Pressure Metering and High Pressure Delivery e Solvent Compressibility Compensation e Variable Stroke Volume e Column Flow Measurement and Control Low pressure solvent metering and high pressure solvent delivery are accomplished by two pump channels each capable of delivering a maximum of 2 5 ml min flow at up to 400 bar pressure Each channel consists of an identical independently controlled pump unit Each pump unit includes a pump metering drive assembly and pump head assembly The pamphlet assemblies both consist of two identical chambers pistons and seals plus an active inlet valve and an outlet ball valve The channel flow outputs are initially joined by a low volume pre mixer and are then connected by a capillary coil to a pressure pulse damper The pressure pulse damper also serves as a pressure transducer which sends system pressure information to the user interface The flow output of the pressure pulse damper is connected to a mixer The standard mixer is a stainless steel tube filled with stainless steel balls The mixer is where mo
5. Parts required Part number Description Other modules G1376 68705 Parts from accessory kit see Accessory Kit Contents Capillary Pump on page 33 2 wrenches 1 4 5 16 inch for capillary connections Preparations Pump is installed in the LC system WARNING When opening capillary or tube fittings solvents may leak out The handling of toxic and hazardous solvents and reagents can hold health risks gt Please observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the solvent vendor especially when toxic or hazardous solvents are used 1 Remove the front cover by pressing the snap fasteners on both sides Figure 9 Removing the Front Cover 42 1200 Series Capillary Pump User Manual Installing the Pump 3 Place the solvent cabinet on top of the capillary pump Place the bottles into the solvent cabinet and place a bottle head assembly into each bottle Connect the solvent tubes from the bottle head assemblies to the inlet connectors Al A2 B1 and B2 of the solvent selection valve and label the tubes accordingly Fix the tubes in the clips of solvent cabinet and capillary pump Using a piece of sanding paper connect the waste tubing to the EMPV and place it into your waste system If the micro pump is not part of a Agilent 1200 System stack or placed on the bottom of a stack connect the corr
6. the mixtures can be linearly interpolated from known values of the single solvents end edited to a new table Unknown isocratic solvent mixtures can be calibrated by setting the calibration table to aqueous aqueous non calibrated and determining the flow rate by volumetric measurement e g filling a calibrated glass syringe for 5 to 10 min Afterwards the response factor is calculated according the following equation Calibration factor entered flow measured flow Example for Chloroform Methanol Entered flow 15 ul min Measured flow 35 ul min Calibration factor 15 ul min 35 ul min 0428 Enter this calibration factor into a calibration table and save it 6 111 6 Troubleshooting and Diagnostics EMPV Test EMPV Test Description The test is designed to verify the performance of the EMPV The test must always be done when the EMPV valve is exchanged The test should also be done if column flow stability problems occur micro mode only The EMPYV test is not a substitute for the leak test or pressure test The leak and pressure tests should also be done when leaks within the pump heads might be the problem The test starts with a short flushing sequence and a cleaning procedure for the EMPV Afterwards low and high pressure is controlled by the EMPV and the appropriate current is monitored Finally a linear pressure ramp is performed Running the EMPV Test 1 Fill vacuum degasser with A1 aqueous solvent
7. zero solvent counter 81 ESD electrostatic discharge strap 118 ESD wrist strap 33 exchanging active inlet valve 126 126 active inlet valve 123 interface board 144 internal parts 116 outlet ball valve sieve 130 188 outlet ball valve 130 hexagonal key 4mm 136 139 142 outlet ball valve sieve 123 hexagonal key 4mm 134 outlet ball valve 123 high pressure pump main board pistons 123 139 HPM 19 pump seals 123 136 hints for successful use 50 purge valve frit 132 humidity 27 purge valve frit 123 hydraulic path parts 150 purge valve 123 132 hydraulic system 28 solvent selection valve 132 wash seals 123 141 141 l external contact cable 159 172 index limit 91 index adjustment 92 F index missing 92 fan failed 80 indicator status 72 features initialization failed 93 GLP 29 inlet valve fuse 85 instrument layout 18 inlet valve missing 88 safety and maintenace 29 installation pump module 37 flow sensor calibration 109 installation flow sensor parts 154 power considerations 25 flow cell 184 power cords 24 solvent information 184 instrument check 56 flow connections 42 instrument status indicator 73 flow precision 28 interface board 144 flow range 28 interface cable 39 frequency range 20 27 internet 186 frit 132 introduction tothe pump 8 fuse 20 L G laboratory bench 26 GPIB connector 20 lamp instrument status 73 GPIB lamp power supply 72 cable 159 lamp status 72 LAN H cable 159 171 hexkey set 33 leak sen
8. 03394 60600 3396 Series Il 3395A integrator see details in section Remote Cables on page 163 3396 Series III 3395B integrator 03396 61010 HP 1050 modules HP 1046A FLD 5061 3378 HP 1046A FLD 5061 3378 Agilent 35900A A D converter 5061 3378 HP 1040 diode array detector 01046 60202 HP 1090 liquid chromatographs 01046 60202 Signal distribution module 01046 60202 BCD cables 3396 integrator 03396 60560 General purpose spade Lugs G1351 81600 Auxiliary Agilent 1100 Series vacuum degasser G1322 61600 158 1200 Series Capillary Pump User Manual Identifying Cables 9 Type Description Part Number CAN cables Agilent 1100 1200 module to module 0 5m Ig 5181 1516 Agilent 1100 1200 module to module 1m Ig 5181 1519 External Agilent 1100 1200 Series interface board to general G1103 61611 contacts purpose GPIB cable Agilent 1100 1200 module to ChemStation 1 m 10833A Agilent 1100 1200 module to ChemStation 2 m 10833B RS 232 cable Agilent 1100 1200 module to a computer 34398A This kit contains a 9 pin female to 9 pin female Null Modem printer cable and one adapter LAN cable Twisted pair cross over LAN cable shielded 3m long for 5023 0203 point to point connection Twisted pair cross over LAN cable shielded 7m long for 5023 0202 point to point connection 1200 Series Capillary Pump User Manual 159 9 Identifying Cables Analog Cables One end of these cables provides a BNC connector to be connected to Agile
9. 20 seconds the error message is generated Probable cause Suggested actions 1 Pump head not installed correctly screws Install the pump head correctly Ensure nothing not secured or pump head not seated e g capillary is trapped between the pump correctly head and body 2 Broken plunger Exchange the plunger Index Limit Index Limit Pump channel A B Index Limit Pump channel B The time required by the plunger to reach the encoder index position was too short pump During initialization the first plunger is moved to the mechanical stop After reaching the mechanical stop the plunger reverses direction until the encoder index position is reached If the index position is reached too fast the error message is generated Probable cause Suggested actions 1 Irregular or sticking drive movement Remove the pump head and examine the seals plungers and internal components for signs of wear contamination or damage Exchange components as required 2 Defective pump drive assembly Exchange the pump drive assembly 1200 Series Capillary Pump User Manual 91 92 Troubleshooting and Diagnostics Index Adjustment Index Adjustment Pump channel A B Index Adjustment Pump channel B The encoder index position in the module is out of adjustment During initialization the first plunger is moved to the mechanical stop After reaching the mechanical stop the plunger reverses direction until the encoder index position is
10. 200 nl Column Temperature 25 0 C or ambient Agilent 1200 Series Capillary LC Degasser Instrument Capillary pump 20 pl minute sensor installed Micro Autosampler Column Compartment optional Detector DAD with 500 nL flow cell installed ChemStation Controlling Software Chemstation EZ Chrom OL etc Column ZORBAX SB C18 5 pm 150 x 0 5 mm Agilent Part No 5064 8256 Standard Agilent Part No 01080 68704 0 15 wt dimethylphthalate 0 15 wt diethylphthalate 0 01 wt biphenyl 0 03 wt o terphenyl in methanol Diluted 1 10 in Acetonitrile 1200 Series Capillary Pump User Manual Using the Capillary Pump 4 For instrument configurations other than shown above the conditions are altered to match the specifications of the instrument Procedure 1 Make a single injection of the isocratic test standard under the conditions given below 2 Compare the resulting chromatogram with the typical chromatogram shown in Figure 11 on page 57 Typical Chromatogram A typical chromatogram for this analysis is shown in Figure 11 on page 57 The exact profile of the chromatogram will depend on the chromatographic conditions Variations in solvent quality column packing standard concentration and column temperature will all have a potential effect on peak retention and response Figure 11 Chromatogram 1200 Series Capillary Pump User Manual 57 4 Using the Capillary Pump Inject the Check out Sample 58 1200 Series Capillary
11. 8 Purge the capillary pump see Priming your capillary LC system with the pump on page 46 NOTE The pump was shipped with default configuration settings To change these settings see configuring the capillary pump in the service manual 1200 Series Capillary Pump User Manual 39 3 Installing the Pump Connecting Modules and Control Software WARNING Use of unsupplied cables Using cables not supplied by Agilent Technologies can lead to damage of the electronic components or personal injury gt Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations Connecting Agilent 1200 Series modules 1 Place the individual modules in a stack configuration as shown in Figure 5 on page 35 2 Ensure the power switches on the front of the modules are OFF switches stand out 3 Plug a CAN cable into the CAN connector at the rear of the respective module except vacuum degasser 4 Connect the CAN cable to the CAN connector of the next module see Figure 6 on page 36 5 Press in the power switches to turn on the modules Connecting an Agilent 1200 Series Vacuum Degasser 1 Place the vacuum degasser in the stack of modules as shown in Figure 5 on page 35 2 Ensure the power switch on the front of the vacuum degasser is OFF switch stands out 3 Plug an APG cable into the APG remote connector at the rear of the module 4 Connec
12. Add a small of organic solvents e g acetonitrile or methanol 5 Use of Solvents Observe the following recommendations on the use of solvents e Brown glass ware can avoid growth of algae e Small particles can permanently block capillaries and valves Therefore always filter solvents through 0 4 um filters e Avoid the use of the following steel corrosive solvents Solutions of alkali halides and their respective acids for example lithium iodide potassium chloride and so on High concentrations of inorganic acids like sulfuric acid and nitric acid especially at higher temperatures if your chromatography method allows replace by phosphoric acid or phosphate buffer which are less corrosive against stainless steel Halogenated solvents or mixtures which form radicals and or acids for example 2CHCly O gt 2COCl 2HC1 This reaction in which stainless steel probably acts as a catalyst occurs quickly with dried chloroform if the drying process removes the stabilizing alcohol 1200 Series Capillary Pump User Manual Appendix 10 Chromatographic grade ethers which can contain peroxides for example THF dioxane di isopropylether such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides Solvents containing strong complexing agents e g EDTA Mixtures of carbon tetrachloride with 2 propanol or THF 1200 Series Capillary Pump User Manual 185 10 Appendix Agilent T
13. Maintenance Removing and Disassembling the Pump Head Assembly When Exchanging pump seals Exchanging plungers Exchanging seals of the seal wash option Wrench 1 4 inch 3 mm hexagonal key Tools required 4 mm hexagonal key Preparations Switch off capillary pump at power switch Remove the front cover to have access to the pump mechanics Damage of the pump drive CAUTION Starting the pump when the pump head is removed may damage the pump drive gt Never start the pump when the pump head is removed 1 Disconnect the capillary at the pumphead adapter and the tube at the active inlet valve Beware of leaking solvents Disconnect the active inlet valve cable plug AN 2 Using a 4 mm hexagonal key step wise loosen and remove the two pump head screws and remove the pump head from the pump drive 7 amp Active inlet valve to mixer Plug Pumphead screws 134 1200 Series Capillary Pump User Manual Maintenance 7 3 Place the pump head on a flat surface Loosen the lock screw two revolutions While holding the lower half of the assembly carefully pull the pump head away from the plunger housing Pump head Lock screw ee GE X LAD DSS ai L 4 Remove the support rings from the plunger housing and lift the housing away from the plungers Plunger housing Plunger 1200 Series Capillary Pump User Manual 135 7 Maintenance Exchanging the Pump S
14. Pump User Manual 1200 Series Capillary Pump User Manual 5 Optimizing Performance Hints for the Micro Vacuum Degasser 60 When to Use Alternative Seals 61 How to Choose the Primary Flow 62 Static Mixer and Filter 64 How to Optimize the Compressibility Compensation Setting 65 gy Agilent Technologies 59 5 Optimizing Performance Hints for the Micro Vacuum Degasser If you are using the vacuum degasser for the first time if the vacuum degasser was switched off for any length of time for example overnight or if the vacuum degasser lines are empty you should prime the vacuum degasser before running an analysis The vacuum degasser can be primed by pumping solvent with the capillary pump at high flow rate 2 5 ml min Priming the degasser is recommended when e vacuum degasser is used for the first time or vacuum chambers are empty e changing to solvent that are immiscible with the solvent currently in the vacuum chambers e capillary pump was turned OFF for a length of time for example during night and volatile solvent mixtures are used For more information see the Reference Manual for the Agilent 1200 series micro vacuum degasser 60 1200 Series Capillary Pump User Manual Optimizing Performance 5 When to Use Alternative Seals The standard seal for the pump can be used for most applications However applications that use normal phase solvents for example hexane are not suited for the standard seal a
15. User Manual 7 127 7 Maintenance When Tools required Parts required 128 Replacing the Active Inlet Valve If internally leaking backflow Wrench 14 mm Part number Description 1 G1312 60025 Active inlet valve body 1 5062 8562 Valve cartridge 400 bar 1 Insert the new valve into the pump head Using the 14 mm wrench turn the nut until it is hand tight 2 Position the valve so that the solvent inlet tube connection points towards the front 3 Using the 14 mm wrench tighten the nut by turning the valve in its final position not more than a quarter turn Do not overtighten the valve The solvent inlet tube connection should point to the right corner of the pump head 4 Reconnect the inlet tube and the active inlet valve cable to the connector at the Z panel Make sure you are in normal mode 1200 Series Capillary Pump User Manual Maintenance 7 Simple Repair Procedures 5 After an exchange of the valve cartridge it may take several mL of pumping with the solvent used in the current application before the flow stabilizes at A ripple as low as it used to be when the system was still working properly Solvent inlet tube Active inlet valve Figure 16 Exchanging the Active Inlet Valve 1200 Series Capillary Pump User Manual 129 7 Maintenance Exchanging the Outlet Ball Valve Sieve or the Complete Valve When Sieve whenever the pump seals will be exchanged Valve if internally leaking T
16. damper to mixer capillary at the damper upper port Disconnect the mixer to filter capillary at the mixer Connect the capillary from the filter into the upper port of the damper nn Oo of FF WwW ND Connect the mixer with the capillary to the flow sensor outlet Position the mixer into a vertical position The flow inlet must be up 8 Pump pure water channel A2 at 1000 ul min normal mode for at least 10 min Be sure the whole pump and mixer is flushed sufficiently Keep an eye on the waste 9 Connect a column at the outlet of the mixer which provides a pressure of 30 to 200 bar at 15 ul min water e g 150 x 0 3 x 5um or a restriction capillary e g Fused silica 50 um ID 2 5 m 10 Pump pure water channel A2 at 15 ul min micro mode until the pressure is absolutely stable at least 5 min 11 Set the compressibility for Al and B1 12 Execute the calibration The flow sensor responses for the composition steps are stored in a file and plotted on the screen 13 Take an average reading of each step and enter it into the calibration table 14 Save the calibration table 15 Remove the column or the restriction capillary and the mixer at the flow sensor outlet 16 Re install the mixer between the damper and the filter 1200 Series Capillary Pump User Manual 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics For water non miscible solvents like Hexane or isopropanol the corresponding values for
17. drive circuits is too high The processor continually monitors the temperature of the drive circuits on the main board If excessive current is being drawn for long periods the temperature of the circuits increases If the temperature exceeds the upper limit the error message is generated Probable cause Suggested actions 1 High friction partial mechanical blockage in Ensure the capillaries and frits between the the pump drive assembly pump head and damper inlet are free from blockage 2 Partial blockage of the flowpath in front of Ensure the outlet valve is not blocked the damper 3 Defective pump drive assembly Remove the pump head assembly Ensure there is no mechanical blockage of the pump head assembly or pump drive assembly Exchange the pump drive assembly 4 Defective main board Exchange the main board 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Motor Drive Power Motor Drive Power Pump channel A B Motor Drive Power Pump channel B The current drawn by the pump motor exceeded the maximum limit Blockages in the flow path are usually detected by the pressure sensor in the damper which result in the pump switching off when the upper pressure limit is exceeded If a blockage occurs before the damper the pressure increase cannot be detected by the pressure sensor and the module will continue to pump As pressure increases the pump drive draws more current When the current r
18. during the intake stroke of piston 1 The active inlet valve is electrically opened and closed making its operation more precise at low pressures The stroke volume of piston 1 is between 2 ul and 100 ul depending on flow rate When the capillary pump is first turned on the user is prompted to initialize the pump The initialization routine occurring for both pump heads first determines the precise movement limits for both pistons These limits are then stored in the pump controller memory Then both pistons are set to their default initial positions When pumping begins the active inlet valve is opened and piston 1 begins its intake stroke sucking solvent into chamber 1 At the same time piston 2 begins its delivery stroke pumping high pressure the existing solvent in chamber 2 out of the pump head The pressure produced by piston 2 also 1200 Series Capillary Pump User Manual Introduction to the Capillary Pump 1 Introduction to the Capillary Pump closes the outlet ball valve preventing any chamber 2 solvent from back streaming into chamber 1 After a predefined piston 1 stroke length the servo motor is stopped and the active inlet valve is closed The pistons now reverse directions Piston 1 begins its delivery stroke high pressure and piston 2 begins its intake stroke Piston 2 is moving at only half the speed of piston 1 The outlet ball valve is forced open by the pressure generated by piston 1 Piston 1 begins to deliver t
19. is not compatible with connecting G1530 60600 printers and plotters RS 232 cable kit 9 to 9 pin female and one adapter 9 pin 34398A male 25 pin female Suited for instrument to PC Cable Printer Serial amp Parallel is a SUB D 9 pin female vs 5181 1529 Centronics connector on the other end NOT FOR FW UPDATE This kit contains a 9 pin female to 9 pin female Null Modem 34398A printer cable and one adapter Use the cable and adapter to connect Agilent Technologies instruments with 9 pin male RS 232 connectors to most PCs or printers 1200 Series Capillary Pump User Manual 173 9 Identifying Cables RS 232 Cable Kit 174 1200 Series Capillary Pump User Manual 1200 Series Capillary Pump User Manual 10 Appendix General Safety Information 176 The Waste Electrical and Electronic Equipment Directive 180 Lithium Batteries Information 181 Radio Interference 182 Sound Emission 183 Solvent Information 184 Agilent Technologies on Internet 186 ee Agilent Technologies 175 10 Appendix General Safety Information General Safety Information The following general safety precautions must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design manufacture and intended use of the instrument Agilent Technologies assumes no liability for the customer s failur
20. of 10 5063 6598 Tube screw pack of 10 5063 6599 Bottle transparent 9301 1420 Bottle amber 9301 1450 Figure 23 Solvent Cabinet Parts 1200 Series Capillary Pump User Manual 149 Parts and Materials for Maintenance Hydraulic Path 150 Table 15 Hydraulic Path Item Description Part Number 1 SF wo N Bottle head assembly Connection tube Capillary outlet ball valve to piston 2 Restriction capillary Mixing capillary Capillary damper to mixer Mixer Capillary mixer to filter Filter assembly includes frit Frit Capillary Filter to EMPV Capillary EMPV to flow sensor 20 ul Capillary EMPV to flow sensor 100 pl Capillary flow sensor to injection device 20 pl Capillary flow sensor to injection device 100 ul Corrugated waste tube 120 cm re order 5 m G1311 60003 G1311 67304 G1312 67300 G1312 67304 G1312 67302 01090 87308 G1312 87330 01090 87308 5064 8273 5022 2185 G1375 87400 G1375 87301 G1375 87305 G1375 87310 G1375 87306 5062 2463 1200 Series Capillary Pump User Manual Parts and Materials for Maintenance 8 Hydraulic Path 10 HH Figure 24 Hydraulic Path 1200 Series Capillary Pump User Manual 151 8 Parts and Materials for Maintenance Pump Head Assembly Table 16 Pump Head Assembly Item Description Part Number Complete assembly included items marked with G1311 60004 1 Sapphire plunger 5063 6586 2 Plunger housing inc
21. reached If the time to reach the index position is too long the error message is generated Probable cause Suggested actions 1 Irregular or sticking drive movement Remove the pump head and examine the seals plungers and internal components for signs of wear contamination or damage Exchange components as required 2 Defective pump drive assembly Exchange the pump drive assembly Index Missing Index Missing Pump channel A B Index Missing Pump channel B The encoder index position in the module was not found during initialization During initialization the first plunger is moved to the mechanical stop After reaching the mechanical stop the plunger reverses direction until the encoder index position is reached If the index position is not recognized within a defined time the error message is generated Probable cause Suggested actions 1 Disconnected or defective encoder cable Ensure the encoder cable are not damaged or dirty Make sure the cables are connected securely to the main board 2 Defective pump drive assembly Exchange the pump drive assembly 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Stroke Length Stroke Length Pump channel A B Stroke Length Pump channel B The distance between the lower plunger position and the upper mechanical stop is out of limits pump During initialization the module monitors the drive current If the plunger reaches the upper mechanical
22. shock and e the metal inner cabinet shields the internal electronics from electromagnetic interference and also helps to reduce or eliminate radio frequency emissions from the instrument itself 1200 Series Capillary Pump User Manual Introduction to the Capillary Pump 1 The Electronics The electronics are comprised of four main components The capillary separation main board CSM e Power supply Optional e Interface board BCD external contacts LAN Communication Interface Board Capillary Separation Main Board CSM The board controls all information and activities of all assemblies within the capillary pump The operator enters parameters changes modes and controls the capillary pump through interfaces CAN GPIB or RS 232C connected to the user interfaces The Main Power Supply Assembly The main power supply comprises a closed assembly no component level repair possibility The power supply provides all DC voltages used in the binary pump module The line voltage can vary in a range from 100 120 or 220 240 volts AC 10 and needs no manual setting Optional Interface Boards The Agilent 1200 Series modules have one optional board slot that allows addition of an interface board to the modules Optional interface boards for the Agilent 1200 Series are BCD Board LAN Communication Interface Board 1200 Series Capillary Pump User Manual 19 1 Introduction to the Capillary Pump E
23. stop position before expected the motor current increases as the module attempts to drive the plunger beyond the mechanical stop This current increase causes the error message to be generated Probable cause Suggested actions 1 Defective pump drive assembly Exchange the pump drive assembly Initialization Failed Initialization Failed Pump channel A B Initialization Failed Pump channel B The module failed to initialize successfully within the maximum time window A maximum time is assigned for the complete pump initialization cycle If the time is exceeded before initialization is complete the error message is generated Probable cause Suggested actions 1 Blocked active inlet valve Exchange the active inlet valve 2 Defective pump drive assembly Exchange the pump drive assembly 3 Defective main board Exchange the main board 1200 Series Capillary Pump User Manual 93 94 Troubleshooting and Diagnostics Wait Timeout When running certain tests in the diagnostics mode or other special applications the pump must wait for the plungers to reach a specific position or must wait for a certain pressure or flow to be reached Each action or state must be completed within the timeout period otherwise the error message is generated Possible Reasons for a Wait Timeout Pressure not reached Pump channel A did not reach the delivery phase Pump channel B did not reach the delivery phase Pump channel A did not r
24. this electrical electronic product in domestic household waste Product Category With reference to the equipment types in the WEEE Directive Annex I this product is classed as a Monitoring and Control Instrumentation product s Do not dispose off in domestic household waste To return unwanted products contact your local Agilent office or see www agilent com for more information 180 1200 Series Capillary Pump User Manual Appendix 10 Lithium Batteries Information Lithium batteries may not be disposed off into the domestic waste Transportation of discharged Lithium batteries through carriers regulated by IATA ICAO ADR RID IMDG is not allowed Danger of explosion if battery is incorrectly replaced gt Discharged Lithium batteries shall be disposed off locally according to national waste disposal regulations for batteries gt Replace only with the same or equivalent type recommended by the equipment manufacturer Lithiumbatteri Eksplosionsfare ved fejlagtig h ndtering Udskiftning ma kun ske med batteri af samme fabrikat og type gt Lever det brugte batteri tilbage til leverand ren Lithiumbatteri Eksplosionsfare Ved udskiftning benyttes kun batteri som anbefalt av apparatfabrikanten gt Brukt batteri returneres appararleverandoren Bij dit apparaat zijn batterijen geleverd Wanneer deze leeg zijn moet u ze niet weggooien maar inleveren als KCA 1200 Series Capillary Pump
25. valve in the module is missing or defective The processor checks the presence of the active inlet valve connector every 2 seconds If the connector is not detected by the processor the error message is generated Probable cause 1 Disconnected or defective cable 2 Disconnected or defective connection cable front panel to main board 3 Defective active inlet valve Suggested actions Ensure the pins of the active inlet valve connector are not damaged Ensure the connector is seated securely Ensure the connection cable is seated correctly Exchange the cable if defective Exchange the active inlet valve 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Electro Magnetic Proportional Valve EMPV Missing EMPV Missing The EMPV in the micro pump is missing or defective Probable cause Suggested actions 1 Disconnected or defective cable Ensure the connection cable is seated correctly 2 Defective solenoid Exchange the solenoid of the EMPV Flow Sensor Missing Probable cause Suggested actions 1 Flow sensor disconnected Ensure the sensor is seated correctly 2 Defective flow sensor Exchange the flow sensor Leak Sensor Missing Probable cause Suggested actions 1 Disconnected or defective cable Ensure the connection cable is seated correctly 2 Defective leak sensor Exchange the leak sensor 1200 Series Capillary Pump User Manual 89 90 Troubleshooting and Diagnostics Servo R
26. 0 bar 2 Before starting the optimization procedure the flow must be stable Use degassed solvent only Check the tightness of the system with the pressure test 3 Your pump must be connected to a control software e g ChemStation EZChrom OL etc or handheld controller with which the pressure and ripple can be monitored otherwhise connect a signal cable between the pressure output of the pump and a recording device for example 339X integrator and set parameters Zero 50 Att 2 3 Chart Speed 10 cm min 4 Start the recording device with the plot mode 1200 Series Capillary Pump User Manual 65 5 Optimizing Performance 5 Starting with a compressibility setting of 10 x 10 bar increase the value in steps of 10 Re zero the integrator as required The compressibility compensation setting that generates the smallest pressure ripple is the optimum value for your solvent composition 6 Repeat step 1 on page 65 through step 5 on page 66 for the B channel of your capillary pump Table9 Solvent Compressibility Solvent pure Compressibility 10 6 bar Acetone 126 Acetonitrile 115 Benzene 95 Carbon tetrachloride 110 Chloroform 100 Cyclohexane 118 Ethanol 114 Ethyl acetate 104 Heptane 120 Hexane 150 Isobutanol 100 Isopropanol 100 Methanol 120 i Propanol 100 Toluene 87 THF 95 Water 46 66 1200 Series Capillary Pump User Manual 1200 Series Capillary Pump User Manual 6 Troubleshooting and Diagnostics Agi
27. 000 5022 2112 5042 8590 G1361 60000 G1376 60001 G1376 60002 1200 Series Capillary Pump User Manual Parts and Materials for Maintenance 8 Pump Housing and Main Assemblies as a T O 4 UOS f p PANS 7 y Y er RS Y DP a i A Figure 21 Overview of Main Assemblies Front View 1200 Series Capillary Pump User Manual 147 8 Parts and Materials for Maintenance Pump Housing and Main Assemblies Table 13 Repair Parts Pump Housing and Main Assemblies Rear View Item Description Part Number 1 Hexagonal nut for RS 232C connector 1251 7788 2 Nut M14 analog output 2940 0256 3 Screw M14 7 mm lg power supply 0515 0910 4 Standoff GPIB connector 0380 0643 mr N S paan F aes F as ff en fo Figure 22 Overview of Main Assemblies Rear View 148 1200 Series Capillary Pump User Manual Parts and Materials for Maintenance 8 Solvent Cabinet and Bottle Head Assembly Table 14 Solvent Cabinet and Bottle Head Assembly Parts Item Description Part Number 1 Solvent cabinet including all plastic parts 5065 9981 2 Name plate Agilent 1200 5042 8901 3 Front panel solvent cabinet 5065 9954 4 Leak pan solvent cabinet 5042 8567 Bottle head assembly for Capillary pump includes items 8 9 10 G1311 60003 and 11 5 6 Solvent inlet filter SST 01018 60025 7 Solvent tubing 5 m 5062 2483 Ferrules with lock ring pack
28. 1 Defective solvent selection valve Restart the capillary pump If the error message appears again exchange the solvent selection valve 2 Defective connection cable front panel to Exchange the connection cable main board 3 Defective main board Exchange the main board Inlet Valve Fuse Inlet Valve Fuse 0 Pump channel A Inlet Valve Fuse 1 Pump channel B One of the active inlet valves in the module has drawn excessive current causing the inlet valve electronic fuse to open Probable cause Suggested actions 1 Defective active inlet valve Restart the module If the error message appears again exchange the active inlet valve 2 Defective connection cable front panel to Exchange the connection cable main board 3 Defective main board Exchange the main board 1200 Series Capillary Pump User Manual 85 86 Troubleshooting and Diagnostics Temperature Out of Range Temperature Out of Range 0 Pump channel A Temperature Out of Range 1 Pump channel B One of the temperature sensor readings in the motor drive circuit are out of range The values supplied to the ADC by the hybrid sensors must be between 0 5 V and 4 3 V If the values are outside this range the error message is generated Probable cause Suggested actions 1 Defective main board Exchange the main board Temperature Limit Exceeded Temperature Limit Exceeded 0 Pump channel A Temperature Limit Exceeded 1 Pump channel B The temperature of one of the motor
29. 1200 module to module 1 m 5181 1519 Agilent 1200 module to control module G1323 81600 LAN Cables Description Part number Cross over network cable shielded 3 m long for point to 5023 0203 point connection Twisted pair network cable shielded 7 m long for hub 5023 0202 connections 1200 Series Capillary Pump User Manual 171 9 Identifying Cables External Contact Cable 109 lt 6 case ono Oly One end of this cable provides a 15 pin plug to be connected to Agilent 1200 Series module s interface board The other end is for general purpose Agilent 1200 Series Interface Board to general purposes Connector G1103 61611 Color Pin Agilent Signal Name 1200 White 1 EXT 1 a Brown 2 EXT 1 Green 3 EXT 2 Bea Yellow 4 EXT 2 Grey 5 EXT 3 Pink 6 EXT 3 Blue 7 EXT 4 Red 8 EXT 4 Black 9 Not connected Violet 10 Not connected Grey pink 11 Not connected Red blue 12 Not connected White green 13 Not connected Brown green 14 Not connected White yellow 15 Not connected 172 1200 Series Capillary Pump User Manual Identifying Cables 9 RS 232 Cable Kit This kit contains a 9 pin female to 9 pin female Null Modem printer cable and one adapter Use the cable and adapter to connect Aligent Technologies instruments with 9 pin male RS 232 connectors to most PCs or printers Description Part number RS 232 cable instrument to PC 9 to 9 pin female This cable 24542U has special pin out and
30. 6 inch 8710 0806 2 ESD wrist strap 9300 1408 1 Hex key 3mm 8710 2411 1 Hex key 2 5 mm 8710 2412 1 Waste tube 0890 1760 2m 1 ESD Electrostatic Discharge 1200 Series Capillary Pump User Manual 33 3 Installing the Pump Optimizing the Stack Configuration 34 If your capillary pump is part of a complete 1200 series system you can ensureoptimum performance by limiting the configuration of the system stack to the following configuration This configuration optimizes the system flow path ensuring minimum delay volume For a detailed view of the flow connections refer to the section Flow connections in chapter 1 of the product information of the individual modules If a single stack configuration becomes too high e g if an additional module like a G1327A ALS Thermostat is added or if your bench is too high a two stack configuration may be a better setup Separate the stack between pump and autosampler and place the stack containing the pump on the right side of the stack containing the autosampler 1200 Series Capillary Pump User Manual Installing the Pump 3 Optimizing the Stack Configuration Solvent cabinet Vacuum degasser Instant pilot Autosampler Column compartment Detector Figure 5 Recommended Stack Configuration Front View 1200 Series Capillary Pump User Manual 35 3 Installing the Pump Optimizing the Stack Configuration AC power Analog signal to recorder Remote
31. 79 composition precision 28 compressibility compensation 28 65 1200 Series Capillary Pump User Manual condensation 26 connections flow 42 control software 41 control software 41 counter seal wear 120 counter EMF 119 D damaged packaging 32 damaged parts 32 delay volume 34 delivery checklist 32 Diagnostic software 69 dimensions 27 disassembling the pump head 134 E early maintenance feedback EMF 18 electrical connections 20 electronic fuses 20 electronic waste 180 electronics CSM board 19 electronics HPM board 19 electrostatic discharge ESD 117 144 EMF flag 119 EMF limits 120 EMF counters 119 EMPV cleaning procedure 113 EMPV test 112 encoder missing 88 environment 26 error condition 73 error messages 70 75 187 Index error messages compensation sensor open 79 compensation sensor short 79 encoder missing 88 fan failed 80 ignition without cover 80 80 index adjustment 92 index limit 91 index missing 92 initialization failed 93 inlet valve fuse 85 inlet valve missing 88 eak sensor open 78 eak sensor short 78 eak 77 missing pressure reading 84 motor drive power 87 pressure above upper limit 82 pressure below lower limit 82 pump head missing 91 remote timeout 76 selection valve failed 83 selection valve fuse 85 servo restart failed 90 shut down 76 stroke length 93 temperature limit exceeded 86 temperature out of range 86 timeout 75 error message wait timeout 94 error
32. Agilent 1200 Series Capillary Pump A User Manual m yO ot Agilent Technologies Notices Agilent Technologies Inc 2007 2008 No part of this manual may be reproduced in any form or by any means including elec tronic storage and retrieval or translation into a foreign language without prior agree ment and written consent from Agilent Technologies Inc as governed by United States and international copyright laws Manual Part Number 61376 90012 Edition 11 08 Printed in Germany Agilent Technologies Hewlett Packard Strasse 8 76337 Waldbronn Research Use Only Not for use in Diagnostic Procedures Warranty The material contained in this docu ment is provided as is and is sub ject to being changed without notice in future editions Further to the max imum extent permitted by applicable law Agilent disclaims all warranties either express or implied with regard to this manual and any information contained herein including but not limited to the implied warranties of merchantability and fitness for a par ticular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing use or perfor mance of this document or of any information contained herein Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms the warranty te
33. B1 organic solvent acetonitrile methanol isopropanol etc 2 If vacuum degasser is totally empty use syringe to draw solvent into the vacuum chamber or flush vacuum degasser before test is executed test requires filled degasser chambers 3 Plug the pump outlet with blank nut at EMPV outlet 4 Disconnect the EMPV to flow sensor capillary G1375 87301 at EMPV outlet and plug the EMPV outlet port with blank nut 01080 83202 5 Execute test 6 Remove the blank nut 7 Reconnect the EMPV to flow sensor capillary Do not overtighten 112 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 EMPV Cleaning Capillary Pump EMPV Cleaning Description Depending on the application particles can sometimes be collected in the EMPV This fast cleaning routine is designed to remove such particle deposits The routine should always be performed when the EMPV is suspected of being leaky or contaminated with particles The outlet of the EMPV is plugged with an SST blank nut After a short flushing routine the EMPV is closed and the pressure is increased to approximately 380 bar The EMPV is then opened and the pressure is released very quickly This procedure is repeated several times in a sequence Running the Test 1 ow uy OO 1 A Fill vacuum degasser channel Al and B1 with solvents the test requires filled vacuum chambers We recommend that you use channel A with aqueous solvent If you use a different cha
34. HPLC Systems 54 How to Prevent and or Reduce the Algae Problem 55 Inject the Check out Sample 56 Conditions 56 Procedure 57 Typical Chromatogram 57 gy Agilent Technologies 49 4 Using the Capillary Pump Hints for Successful Use of the Capillary Pump 50 Pump issues Flush the pump extensively First with in the purge mode second with a pressure applied to remove all the gas bubbles It is recommended to do this first with 100 A and than 100 B The system pressure must be higher than 20 Bar at the pump outlet In micro mode unexpected high column flow variation is an indication for dirt within the system blocked frits or leaking pump valves Place solvent cabinet with the solvent bottles always on top or at a higher level of the capillary pump Prevent blocking ofsolvent inlet filters never use the pump without solvent inlet filter Growth of algae should be avoided When using buffer solutions flush the system with water before switching it off Check the pump plungers for scratches when changing the piston seals Scratched plungers will lead to micro leaks and will decrease the lifetime of the seal After changing the plunger seals apply the seal wear in procedure Place the aqueous solvent on channel A and the organic solvent on channel B The default compressibility and flow sensor calibration settings are set accordingly Always use the correct calibration values For generation of fast
35. Pump User Manual 137 7 138 Maintenance Seal Wear in Procedure This procedure is required for standard seals only 5063 6589 but it will definitely damage the normal phase application seals 0905 1420 Place a bottle with 100 ml of Isopropanol in the solvent cabinet and place the tubing including bottle head assembly of the pump head that is supposed to be worn in into the bottle Screw the adapter 0100 1847 to the AIV and connect the inlet tube from the bottle head directly to it Connect the restriction capillary 5022 2159 to the outlet of the EMPV Insert its other end into a waste container Turn the system in purge mode and purge the system for 2 minutes with isopropanol at a flow rate of 2 ml min Turn the system to standard mode set the flow to a rate adequate to achieve a pressure of 350 bar Pump 15 minutes at this pressure to wear in the seals The pressure can be monitored at your analog output signal with the handheld controller Chemstation or any other controlling device connected to your pump Turn OFF the pump slowly disconnect the restriction capillary from the EMPYV to release the pressure from the system Reconnect the capillary going to the flow sensor and the connecting tube from solvent selection valve to the AIV Rinse your system with the solvent used for your next application 1200 Series Capillary Pump User Manual Exchanging the Plungers When When scratched Tools required 3 mm
36. T default setting 1 to 99 or 5 l min per channel primary flow whatever is greater lt 0 2 SD at 10 pl min 20 pl flow sensor 50 l min 100 pl flow sensor and 1 ml min normal mode default setting Typically 3 pl from the electronic flow control to the pump outlet for flow rates up to 20 l min Typically 12 pl from the electronic flow control to the pump outlet for flow rates up to 100 yl for flow rates up to 100 pl min and electronic flow control active primary flow path 180 480 pl without mixer 600 900 pl with mixer system pressure dependant Typically 180 to 480 pl system pressure dependent without mixer for flow rates up to 2 5 ml min Mixer delay volume 420 pl 20 to 400 bar 5880 psi system pressure User selectable based on mobile phase compressibility 1 0 8 5 solvents with pH lt 2 3 should not contain acids which attack stainless steel Upper pH range is limited by fused silica capillaries 28 1200 Series Capillary Pump User Manual Site Requirements and Specifications 2 Table4 Performance Specification Agilent 1200 Series Capillary Pump Type Specification Control and data Agilent Control Software Chemstation EZ Chrom OL etc evaluation Analog output For pressure monitoring 2 mV bar one output Communications Controller area network CAN GPIB RS 232C APG Remote ready start stop and shut down signals LAN optional Safety and Extensive diagnostics error detectio
37. Table 3 on page 27 allow to place the module on almost any laboratory bench It needs an additional 2 5 cm 1 0 inches of space on either side and approximately 8 cm 3 1 inches in the rear for the circulation of air and electric connections If the bench should carry a complete Agilent 1200 Series system make sure that the bench is designed to carry the weight of all the modules The module should be operated in a horizontal position Environment Your module will work within specifications at ambient temperatures and relative humidity as described in Table 3 on page 27 CAUTION Condensation within the module Condensation will damage the system electronics gt Do not store ship or use your module under conditions where temperature fluctuations could cause condensation within the module gt If your module was shipped in cold weather leave it in its box and allow it to warm slowly to room temperature to avoid condensation 26 1200 Series Capillary Pump User Manual Site Requirements and Specifications 2 Physical Specifications Table3 Physical Specifications Type Specification Comments Weight 17 kg 38 Ibs Dimensions 180 x 345 x 435 mm 7 x 13 5 x 17 width x depth x height Line voltage Line frequency Power consumption Ambient operating temperature Ambient non operating temperature Humidity Operating Altitude Non operating altitude Safety standards IEC CSA UL inches 100 240
38. Unplug the pump from main power Disconnect cables from the interface board connectors Loosen the screws Slide out the interface board from the capillary pump Install the new interface board Secure screws oa A O N Reconnect the cables to the board connector BCD Interface board Figure 20 Exchanging the Interface Board 144 1200 Series Capillary Pump User Manual 1200 Series Capillary Pump User Manual 8 Parts and Materials for Maintenance Pump Housing and Main Assemblies 146 Solvent Cabinet and Bottle Head Assembly 149 Hydraulic Path 150 Pump Head Assembly 152 Flow Sensor Assembly 154 Capillary Pump Accessory Kit 155 gy Agilent Technologies 145 Parts and Materials for Maintenance Pump Housing and Main Assemblies 146 Table 12 Repair Parts Pump Housing and Main Assemblies Front View Item Description Part Number 1 2 Pump head see Pump Head Assembly on page 152 Pump drive assembly Exchange assembly pump drive Cable assembly AIV to main board Capillary system main board CSM Exchange assembly CSM board Cable assembly solvent selection valve Fan assembly Damping unit Solvent selection valve half of a complete valve Screw solvent selection valve Leak pan pump EMPV Flow Sensor 20 ul Flow Sensor 100 ul G1311 60004 G1311 60001 G1311 69001 G1311 61601 G1376 66530 G1376 69530 G1312 61602 3160 1017 79835 60005 G1312 60
39. User Manual 181 10 Appendix Radio Interference Cables supplied by Agilent Technoligies are screened to provide opitimized protection against radio interference All cables are in compliance with safety or EMC regulations Test and Measurement If test and measurement equipment is operated with unscreened cables or used for measurements on open set ups the user has to assure that under operating conditions the radio interference limits are still met within the premises 182 1200 Series Capillary Pump User Manual Appendix 10 Sound Emission Manufacturer s Declaration This statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991 This product has a sound pressure emission at the operator position lt 70 dB e Sound Pressure Lp lt 70 dB A e At Operator Position e Normal Operation e According to ISO 7779 1988 EN 27779 1991 Type Test 1200 Series Capillary Pump User Manual 183 10 Appendix Solvent Information 184 Flow Cell To protect optimal functionality of your flow cell Avoid the use of alkaline solutions pH gt 9 5 which can attack quartz and thus impair the optical properties of the flow cell If the flow cell is transported while temperatures are below 5 degree C it must be assured that the cell is filled with alcohol Aqueous solvents in the flow cell can built up algae Therefore do not leave aqueous solvents sitting in the flow cell
40. VAC 10 50 or 60 Hz 5 180 VA 75 W 256 BTU 4 to 55 C 41 to 131 F 40 70 C 4 158 F lt 95 at 25 40 C 77 104 F Up to 2000 m 6500 ft Up to 4600 m 14950 ft Installation Category II Pollution Degree 2 Wide ranging capability Maximum Non condensing For storing the module For indoor use only Research Use Only Not for use in Diagnostic Procedures 1200 Series Capillary Pump User Manual 27 2 Site Requirements and Specifications Performance Specifications Table 4 Performance Specification Agilent 1200 Series Capillary Pump Type Specification Hydraulic system Settable column flow range Recommended column flow range Column flow precision Optimum composition range Composition precision Delay volume Pressure range Compressibility compensation Recommended pH range Two dual piston in series with proprietary servo controlled variable stroke drive floating piston active inlet valve solvent selection valve and electronic flow control for flow rates up to 100 l min 0 01 20 pl min 0 01 100 pl min with the extended flow range kit 0 001 2 5 pl min with the electronic flow control bypassed 1 20 pl min 10 100 pl min with extended flow range kit 0 1 2 5 ml min with the electronic flow sensor bypassed lt 0 7 RSD or 0 03 SD typically 0 4 RSD or 0 02 SD at 10 pl min and 50 pl min column flow based on R
41. all valves inlet or outlet resulting in unstable flow or total failure of the pump e Small pore solvent inlet filters to plug resulting in unstable flow or total failure of the pump e Small pore high pressure solvent filters usually placed before the injector to plug resulting in high system pressure e Column filters to plug giving high system pressure e Flow cell windows of detectors to become dirty resulting in higher noise levels since the detector is the last module in the flow path this problem is less common Symptoms Observed with the Agilent 1200 Series HPLC In contrast to the HP 1090 and HP 1050 Series HPLC systems which use helium degassing algae have a better chance to grow in systems such as the Agilent 1200 Series where helium is not used for degassing most algae need oxygen and light for growth The presence of algae in the Agilent 1200 Series can cause the following to occur e PTFE frits part number 01018 22707 purge valve assembly and column filter blockage causing increased system pressure Algae appear as white or yellowish white deposits on filters Typically black particles from the 1200 Series Capillary Pump User Manual Using the Capillary Pump 4 normal wear of the piston seals do not cause the PTFE frits to block over short term usage Please refer to the section Exchanging the Solvent Selection Valve on page 132 in this manual Short lifetime of solvent filters bottle head assemb
42. alve capillary Outlet ball valve Figure 18 Exchanging the Outlet Ball Valve 1200 Series Capillary Pump User Manual 131 7 Maintenance Simple Repair Procedures Exchanging the Solvent Selection Valve When If leaking internally croossflow between the ports or if one of the channels is blocked Tools required Screwdriver Pozidriv 1 Parts required Part number Description 1 G1312 60000 Solvent selection valve PN gives half of a complete solvent selection block 1 Disconnect the solvent tubes and the active inlet valve connection tubes from the solvent selection valves Place solvent tubes into the solvent cabinet to prevent leaks due to hydrostatic flow Solvent tubes ate Solvent selection valve CN N Connecting tubes Figure 19 Exchanging the solvent selection valve 132 1200 Series Capillary Pump User Manual Maintenance 7 2 Using a Pozidriv screwdriver 1 loosen the holding screws of the valves 3 Pull the valve module out of its connector Hold the two plastic bodies of the valves and pull the two solvent selection valves apart 5 Exchange the defective solvent selection valve Press the exchanged valve new half together with the properly working old half 6 Connect the valve module to its electrical connectors and fix the assembly with the two holding screws 7 Reinstall solvent tubes and the active inlet valve connection tubes 1200 Series Capillary Pump User Manual 133 7
43. ary Pump User Manual 1200 Series Capillary Pump User Manual 2 Site Requirements and Specifications Site Requirements 24 Physical Specifications 27 Performance Specifications 28 ee Agilent Technologies 23 2 Site Requirements and Specifications Site Requirements Site Requirements A suitable environment is important to ensure optimal performance of the pump Power Cords Different power cords are offered as options with the module The female end of all power cords is identical It plugs into the power input socket at the rear of the module The male end of each power cord is different and designed to match the wall socket of a particular country or region The absence of ground connection and the use of an unspecified power cord can lead to electric shock or short circuit Electric Shock gt Never operate your instrumentation from a power outlet that has no ground connection gt Never use a power cord other than the Agilent Technologies power cord designed for your region Use of unsupplied cables Using cables not supplied by Agilent Technologies can lead to damage of the electronic components or personal injury gt Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations 24 1200 Series Capillary Pump User Manual Site Requirements and Specifications 2 Power Considerations The power supply of the p
44. ble 8 Primary flow overview for standard pump configuration 0 bar 100 bar 200 bar 300 bar 400 bar System System System System System pressure pressure pressure pressure pressure Low consumption range 200 225 250 275 300 Default range 500 570 640 710 780 Fast gradient range 800 995 1190 1385 1580 62 1200 Series Capillary Pump User Manual Optimizing Performance 5 How to Choose the Primary Flow NOTE In any case the standard configuration is changed the primary flow could be higher compared to the values in above table 1200 Series Capillary Pump User Manual 63 5 Optimizing Performance Static Mixer and Filter The capillary pump is equipped with a static mixer and an inline filter in front of the EMPV The Standard Static Mixer The standard static mixer has a volume of typically 420 ul In order to reduce the delay volume of the pump you can remove the mixer Conditions to remove the static mixer e The delay volume of the pump should be reduced to a minimum for fastest gradient response e The detector is used at medium or low sensitivity Removing the mixer will result in an increase of the composition wander and higher detector noise The Standard Filter The standard filter has a volume of typically 100 ul If the application needs a reduced volume e g for fast gradient the 20 ul low volume filter 01090 68703 is recommended Be aware that the filter efficiency and capacity is significantly reduced com
45. cable AC power CAN Bus cable AC power AC power Analog signal to recorder AC power GPIB or LAN to LC control software Figure 6 Recommended Stack Configuration Rear View 36 1200 Series Capillary Pump User Manual Installing the Pump 3 Installing the Capillary Pump Parts required Preparations Part number Description 1 Pump 1 Power cord for other cables see text below and Cable Overview on page 158 1 G4208A Control Software ChemStation EZChrom OL etc 1 G1323B and or a handheld controller Instant Pilot or Control Module Locate bench space Provide power connections Unpack the pump Module is partially energized when switched off as long as the power cord is plugged in Repair work at the module can lead to personal injuries e g shock hazard when the cover is opened and the module is connected to power gt Make sure that it is always possible to access the power plug gt Remove the power cable from the instrument before opening the cover gt Do not connect the power cable to the Instrument while the covers are removed CAUTION Defective on arrival problems If there are signs of damage please do not attempt to install the module Inspection by Agilent is required to evaluate if the instrument is in good condition or damaged gt Notify your Agilent sales and service office about the damage gt An Agilent service representative will inspect the instrument at your s
46. configured accordingly Probable cause Suggested actions 1 Volume in bottle below specified volume Refill bottles and reset solvent counters 2 Incorrect setting of limit Control setting of limit 1200 Series Capillary Pump User Manual 81 6 82 Troubleshooting and Diagnostics Pressure Above Upper Limit The system pressure has exceeded the upper pressure limit Probable cause 1 Upper pressure limit set too low 2 Blockage in the flowpath after the damper 3 Defective damper 4 Defective main board Pressure Below Lower Limit Suggested actions Ensure the upper pressure limit is set to a value suitable for the analysis Check for blockage in the flowpath The following components are particularly subject to blockage purge valve frit needle autosampler seat capillary autosampler sample loop autosampler column frits and capillaries with low internal diameters e g 0 12 mm id Exchange the damper Exchange the main board The system pressure has fallen below the lower pressure limit Probable cause 1 Lower pressure limit set too high 2 Air bubbles in the mobile phase 3 Leak 4 Defective damper 5 Defective main board Suggested actions Ensure the lower pressure limit is set to a value suitable for the analysis Ensure solvents are degassed Purge the module Ensure solvent inlet filters are not blocked Inspect the pump head capillaries and fittings for signs
47. ctly If there are still signs of a leak exchange the appropriate seal active inlet valve outlet ball valve or EMPV Exchange the pump seals 77 78 Troubleshooting and Diagnostics Leak Sensor Open The leak sensor in the module has failed open circuit The current through the leak sensor is dependent on temperature A leak is detected when solvent cools the leak sensor causing the leak sensor current to change within defined limits If the current falls outside the lower limit the error message is generated Probable cause Suggested actions 1 Leak sensor not connected to the main Ensure the leak sensor is connected correctly board 2 Defective leak sensor Exchange the leak sensor Leak Sensor Short The leak sensor in the module has failed short circuit The current through the leak sensor is dependent on temperature A leak is detected when solvent cools the leak sensor causing the leak sensor current to change within defined limits If the current increases above the upper limit the error message is generated Probable cause Suggested actions 1 Defective leak sensor Exchange the leak sensor 2 Leak sensor incorrectly routed being pinched by a metal component 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Compensation Sensor Open The ambient compensation sensor NTC on the main board in the module has failed open circuit The resistance across the temperature comp
48. demonstrate the leak tightness of the capillary pump The test involves monitoring the pressure profile as the capillary pump runs through a predefined pumping sequence The resulting pressure profile provides information about the pressure tightness and operation of the capillary pump components Ramp 1 The test begins with the initialization of both pumps After initialization plungers Al and B1 are both at the top of their stroke Next the capillary pump begins pumping solvent with a flow rate of 150 l min stroke of 100 ul and a composition of 51 A 49 B Both pumps deliver for one complete pump cycle At the end of this step plungers Al and B1 are at the top of their stroke Ramp 2 The capillary pump continues pumping solvent with a flow rate of 150 ul min Channel A delivers for one pump cycle first plunger A2 delivers then plunger A1 followed by channel B plunger B2 then plunger B1 both channels with a stroke of 20 ul Ramp 3 Just before the start of the first plateau plunger A2 delivers with a flow rate of 50 ul min for approximately 8 seconds Plateau 1 At plateau 1 plunger A2 delivers with a flow rate of 3 ul min for 30 seconds Ramp 4 Plunger B2 delivers 50 ul min for approximately 8 seconds 1200 Series Capillary Pump User Manual 101 6 Troubleshooting and Diagnostics Plateau 2 Plunger B2 delivers with a flow rate of 3 ul min for 30 seconds Ramp 5 Plunger A1 delivers 50 ul min for approx
49. e Color Pin Agilent Signal Name BCD Digit 1200 Green 1 BCD 5 20 Violet 2 BCD 7 80 a Blue 3 BCD 6 40 S Yellow 4 BCD 4 10 oe Black 5 BCD 0 1 Ras Orange 6 BCD 3 8 Red 7 BCD 2 4 Brown 8 BCD 1 2 Gray 9 Digital ground Gray Gray pink 10 BCD 11 800 Red blue 11 BCD 10 400 White green 12 BCD 9 200 Brown green 13 BCD 8 100 notconnected 14 notconnected 15 5V Low 168 1200 Series Capillary Pump User Manual Identifying Cables 9 Agilent 1200 to 3396 Integrators Connector03396 60560 Pin 3392 3 Pin Agilent Signal Name BCD Digit 1200 1 1 BCD 5 20 ae 2 2 BCD 7 80 K 3 3 BCD 6 40 4 4 BCD4 10 g 5 5 BCDO 1 6 6 BCD 3 8 7 7 BCD 2 4 8 8 BCD 1 2 9 9 Digital ground NC 15 5V Low 1200 Series Capillary Pump User Manual 169 9 Identifying Cables Auxiliary Cable 170 One end of this cable provides a modular plug to be connected to the Agilent 1100 Series vacuum degasser The other end is for general purpose Agilent 1100 Series Degasser to general purposes Connector G1322 81600 Color Pin Agilent Signal Name 1100 ee White 1 Ground n Brown 2 Pressure signal Green 3 Yellow 4 Grey 5 DC 5VIN Pink 6 Vent 1200 Series Capillary Pump User Manual Identifying Cables 9 CAN LAN Cables Both ends of this cable provide a modular plug to be connected to Agilent 1200 Series module s CAN or LAN connectors CAN Cables Agilent 1200 module to module 0 5 m 5181 1516 Agilent
50. e fully understood and met A WARNING notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly performed or adhered to could result in personal injury or death Do not proceed beyond a WARNING notice until the indi cated conditions are fully under stood and met 1200 Series Capillary Pump User Manual Contents Contents 1 Introduction to the Capillary Pump 7 Introduction to the Capillary Pump 8 Instrument Layout 18 The Electronics 19 Electrical Connections 20 Agilent 1200 Series Interfaces 22 2 Site Requirements and Specifications 23 Site Requirements 24 Physical Specifications 27 Performance Specifications 28 3 Installing the Pump 31 Unpacking the Capillary Pump 32 Optimizing the Stack Configuration 34 Installing the Capillary Pump 37 Connecting Modules and Control Software 40 Flow Connections of the Capillary Pump 42 Get the System Ready for the First Injection 46 4 Using the Capillary Pump 49 Hints for Successful Use of the Capillary Pump 50 Solvent Information 52 Prevent Blocking of Solvent Filters 53 Algae Growth in HPLC Systems 54 Inject the Check out Sample 56 5 Optimizing Performance 59 Hints for the Micro Vacuum Degasser 60 When to Use Alternative Seals 61 How to Choose the Primary Flow 62 Static Mixer and Filter 64 1200 Series Capillary Pump User Manual Contents How to Optimize the Compressibility Compensation Sett
51. e to comply with these requirements WARNING Ensure the proper usage of the equipment The protection provided by the equipment may be impaired gt The operator of this instrument is advised to use the equipment in a manner as specified in this manual Safety Standards This is a Safety Class I instrument provided with terminal for protective earthing and has been manufactured and tested according to international safety standards 176 1200 Series Capillary Pump User Manual Appendix 10 Operation Before applying power comply with the installation section Additionally the following must be observed Do not remove instrument covers when operating Before the instrument is switched on all protective earth terminals extension cords auto transformers and devices connected to it must be connected to a protective earth via a ground socket Any interruption of the protective earth grounding will cause a potential shock hazard that could result in serious personal injury Whenever it is likely that the protection has been impaired the instrument must be made inoperative and be secured against any intended operation Make sure that only fuses with the required rated current and of the specified type normal blow time delay and so on are used for replacement The use of repaired fuses and the short circuiting of fuse holders must be avoided Some adjustments described in the manual are made with power supplied to the i
52. each the take in phase Pump channel B did not reach the take in phase Solvent volume not delivered within the specified time Probable cause Suggested actions 1 System still in purge mode Ensure that purge valve is closed 2 Leak at fittings EMPV active inlet valve Ensure pump components are seated correctly outlet ball valve or plunger seals If there are still signs of a leak exchange the appropriate seal purge valve active inlet valve outlet ball valve plunger seal 3 Flow changed after starting test Ensure correct operating condition for the special application in use 4 Defective pump drive assembly Exchange the defective pump drive assembly 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Micro Mode Pressure Test Description This is a fast test to verify the tightness of a micro system where the pump is operating in the micro mode and no manual purge valve is installed The flow path of the system which is tested for tightness is blocked by a blank nut The pressure is increased up to 380 bar and the remaining flow is measured in the flow sensor while the system is blocked Step 1 The test begins with the initialization of both pump heads Next pump A begins pumping solvent until a system pressure of 380 bar is reached Step 2 The pump is operating in the pressure control mode at 380 bar for several minutes The remaining flow in the column flow path between the EMPV a
53. eaches the maximum limit the module is switched off and the error message is generated Probable cause Suggested actions 1 Flow path blockage in front of the damper Ensure the capillaries and frits between the pump head and damper inlet are free from blockage 2 Blocked outlet ball valve Exchange the outlet ball valve 3 High friction partial mechanical blockage in Remove the pump head assembly Ensure there the pump drive assembly is no mechanical blockage of the pump head assembly or pump drive assembly 4 Defective pump drive assembly Exchange the pump drive assembly 5 Defective main board Exchange the main board 6 Restriction capillary blocked at pre mixing Exchange restriction capillary union 1200 Series Capillary Pump User Manual 87 88 Troubleshooting and Diagnostics Encoder Missing Encoder Missing Pump channel A B Encoder Missing Pump channel B The optical encoder on the pump motor in the module is missing or defective The processor checks the presence of the pump encoder connector every 2 seconds If the connector is not detected by the processor the error message is generated Probable cause Suggested actions 1 Defective or disconnected pump encoder Ensure the connector is clean and seated connector correctly 2 Defective pump drive assembly Exchange the pump drive assembly Inlet Valve Missing Inlet Valve Missing Pump channel A B Inlet Valve Missing Pump channel B The active inlet
54. eals and Seal Wear in Procedure When Seals leaking if indicated by the results of the pump test check both pump heads individually Tools required 3 mm hexagonal key 4 mm hexagonal key 1 4 inch wrench Parts required Part number Description 2 5063 6589 Seals pack of 2 standard or 0905 1420 for normal phase application 1 5022 2159 For the seal wear in procedure Restriction capillary 1 Disassemble the pump head assembly of the leaky pump 2 Using one of the plungers carefully remove the seal from head see Removing and Disassembling the Pump Head the pump head be careful not to break the plunger Assembly on page 134 Remove wear retainers if still present Plunger 136 1200 Series Capillary Pump User Manual Maintenance 7 Simple Repair Procedures 3 Clean the pump chambers with lint free cloth Ensure all 4 Insert seals into the pump head and press firmly in particulate matter is removed Best cleaning results will position be achieved by removing all valves see Removing the Active Inlet Valve on page 126 and Exchanging the Outlet Ball Valve Sieve or the Complete Valve on page 130 and the capillary Inject solvent into each chamber Chambers 5 Reassemble the pump head assembly see Reassembling the Pump Head Assembly on page 142 Reset theseal wear counter and liquimeter as described in the User Interface documentation 1200 Series Capillary
55. echanically blocked obstructing fan blades Open Cover The top foam has been removed The sensor on the main board detects when the top foam is in place If the foam is removed the fan is switched off and the error message is generated Probable cause Suggested actions 1 The top foam was removed during operation Reinstall the top foam 2 Foam not activating the sensor Replace the top foam 3 Sensor defective Exchange the main board 4 Rear of the module is exposed to strong Ensure that the rear of module is not directly direct sunlight exposed to strong sunlight 80 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Restart Without Cover The module was restarted with the top cover and foam open The sensor on the main board detects when the top foam is in place If the module is restarted with the foam removed the module switches off within 30 s and the error message is generated Probable cause Suggested actions 1 The module started with the top cover and Reinstall the top cover and foam foam removed 2 Rear of the module is exposed to strong Ensure that the rear of module is not directly direct sunlight exposed to strong sunlight zero Solvent Counter Pump firmware version A 02 32 and higher allow to set solvent bottle fillings at the ChemStation revision 5 xx and higher If the volume level in the bottle falls below the specified value the error message appears when the feature is
56. echnologies on Internet For the latest information on products and services visit our worldwide web site on the Internet at http www agilent com Select Products Chemical Analysis It will provide also the latest firmware of the Agilent 1200 Series modules for download 186 1200 Series Capillary Pump User Manual Index Index A accessory kit parts 155 accessory kit 33 active inlet valve 126 126 active inlet valve 123 Agilent Diagnostic software 69 Agilent Lab Advisor software 69 Agilent Lab Advisor 69 Agilent oninternet 186 algae growth 53 algae 50 184 184 alternative seal material 61 ambient operating temperature 27 ambient non operating temperature 27 analog output 20 analog output 29 analog cable 158 160 AUTO mode 16 AUX output 41 auxiliary cable 158 170 battery safety information 181 BCD output 20 BCD board 144 BCD cable 158 168 bench space 26 binary pump checklist 32 blank nut 99 blockage 87 bottle head assembly parts 149 bottle head assembly 32 buffer application 50 C cable analog 158 160 auxiliary 158 170 BCD 158 168 CAN 32 171 external contact 172 external contacts 159 GPIB 159 interface 39 LAN 159 171 power 32 remote 32 158 163 RS 232 159 signal 32 cables overview 158 CAN bus 20 CAN cable 171 capillary separation main board CSM 19 checklist binary pump 32 check out sample 56 cleaning the pump 118 compensation sensor open 79 compensation sensor short
57. el A2 is active To test the pressure tightness of the pump use the leak test see Capillary Pump Leak Test Description on page 101 Step 2 When the system pressure reaches 390 bar the capillary pump switches off The pressure drop from this point onwards should be no more than 2 bar minute Positioning the Blank Nut If a specific component is suspected of causing a system leak place the blank nut immediately before the suspected component then run the pressure test again If the test passes the defective component is located after the blank nut Confirm the diagnosis by placing the blank nut immediately after the suspected component The diagnosis is confirmed if the test fails 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Running the Pressure Test When Tools required Parts required Preparations When problems with leaks are suspected or after maintenance of flow path components e g pump seals injection seal to prove pressure tightness up to 400 bar Wrench 1 4 inch Part number Description 1 01080 83202 Blank nut 500 ml lsopropanol Place a bottle of LC grade isopropanol in the solvent cabinet and connect it to channel A2 Make absolutely sure that all parts of the flow path that are part of the test are very thoroughly flushed with IPA before starting to pressurize the system Any trace of other solvents or the smallest air bubble inside the flow path definitely will cause t
58. ensation sensor NTC on the main board is dependent on ambient temperature The change in resistance is used by the leak circuit to compensate for ambient temperature changes If the resistance across the sensor increases above the upper limit the error message is generated Probable cause Suggested actions 1 Defective main board Exchange the main board Compensation Sensor Short The ambient compensation sensor NTC on the main board in the module has failed short circuit The resistance across the temperature compensation sensor NTC on the main board is dependent on ambient temperature The change in resistance is used by the leak circuit to compensate for ambient temperature changes If the resistance across the sensor falls below the lower limit the error message is generated Probable cause Suggested actions 1 Defective main board Exchange the main board 1200 Series Capillary Pump User Manual 79 6 Troubleshooting and Diagnostics Fan Failed The cooling fan in the module has failed The hall sensor on the fan shaft is used by the main board to monitor the fan speed If the fan speed falls below 2 revolutions second for longer than 5 seconds the error message is generated Probable cause Suggested actions 1 Fan cable disconnected Ensure the fan is connected correctly 2 Defective fan Exchange fan 3 Defective main board Exchange the main board 4 Improperly positioned cables or wires Ensure the fan is not m
59. estart Failed Servo Restart Failed Pump channel A B Servo Restart Failed Pump channel B The pump motor in the module was unable to move into the correct position for restarting When the module is switched on the first step is to switch on the C phase of the variable reluctance motor The rotor should move to one of the C positions The C position is required for the servo to be able to take control of the phase sequencing with the commutator If the rotor is unable to move or if the C position cannot be reached the error message is generated Probable cause Suggested actions 1 Disconnected or defective cables Ensure the pump assembly cables are not damaged or dirty Make sure the cables are connected securely to the main board 2 Mechanical blockage of the module Remove the pump head assembly Ensure there is no mechanical blockage of the pump head assembly or pump drive assembly 3 Defective pump drive assembly Exchange the pump drive assembly 4 Defective main board Exchange the main board 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Pump Head Missing Pump Head Missing Pump channel A B Pump Head Missing Pump channel B The pump head end stop in the pump was not found When the pump restarts the metering drive moves forward to the mechanical end stop Normally the end stop is reached within 20 seconds indicated by an increase in motor current If the end point is not found within
60. et Agilent Lab Advisor provides diagnostic capabilities for all Agilent 1200 Series HPLC modules This includes tests and calibrations procedures as well as the different injector steps to perform all the maintenance routines Agilent Lab Advisor also allows users to monitor the status of their LC instruments The Early Maintenance Feedback EMF feature helps to carry out preventive maintenance In addition users can generate a status report for each individual LC instrument The tests and diagnostic features as provided by the Agilent Lab Advisor Software may differ from the descriptions in this manual For details refer to the Agilent Lab Advisor help files This manual provides lists with the names of Error Messages Not Ready messages and other common issues 1200 Series Capillary Pump User Manual 69 6 Troubleshooting and Diagnostics Overview of the Pump s Indicators and Test Functions Status Indicators The capillary pump is provided with two status indicators which indicate the operational state prerun run and error states of the capillary pump The status indicators provide a quick visual check of the operation of the capillary pump see Status Indicators on page 72 Error Messages In the event of an electronic mechanical or hydraulic failure the instrument generates an error message in the user interface For details on error messages and error handling please refer to the Agilent Lab Monitor amp Diagnos
61. f test procedure is running An error condition is indicated when the status indicator is red An error condition indicates the capillary pump has detected an internal problem which affects correct operation of the instrument Usually an error condition requires attention for example leak defective internal components An error condition always interrupts the analysis A flashing yellow status indicator indicates that the module is in its resident mode Call your local service provider for assistance upon observing this error condition A flashing red status indicator indicates a severe error during the startup procedure of the module Call your local service provider for assistance upon observing this error condition 1200 Series Capillary Pump User Manual 73 6 Troubleshooting and Diagnostics User Interfaces 74 Depending on the User Interface the available test vary Some descriptions are only available in the Service Manual Table 10 Test Functions available vs User Interface Test Micro Mode Pressure Test Normal Mode Pressure Test Leak Test Flow Sensor Solvent Calibration EMPV Test EMPV Cleaning ChemStation Yes Yes Yes Yes Yes Yes Instant Pilot G4208A Yes Yes Yes No No Yes Control Module G1323B Yes Yes Yes Yes Yes Yes Agilent Lab Monitor amp Diagnostic Software Yes Yes Yes Yes Yes Yes 1200 Series Capillary P
62. gradients on short columns remove the mixer enter the new pump configuration and select the fast gradient range for the primary flow rate chromatographic performance will not be impacted When running the Micro mode check the correct instrument setup flow sensor type used mixer and filter Fused Silica Capillary issues When you connect a capillary especially at the column press it smoothly into the fitting to avoid air gaps Incorrect setting will result in dispersion causing tailing or footing peaks 1200 Series Capillary Pump User Manual Using the Capillary Pump 4 Do not overtighten the Fused Silica Capillaries Refer to the capillaries and fittings Chapter in this manual for correct installation e Be careful when you bend a Fused Silica Capillary The diameter must not be smaller than 40 mm 40 mm e When you replace a part especially a capillary clean it with Acetone Ifa fused silica capillary leaks do not retighten under flow Set column flow to zero reinsert the capillary tighten and set new column flow e Avoid the use of alkaline solutions pH gt 8 5 which can attack the fused silica from the capillaries e Be careful not to crush capillaries when applying module doors e A broken capillary can release silica particles into the system e g cell causing problems in the system down stream of the break e A blocked capillary can be often cleaned by flushing it back Acetone is recommended fo
63. he test to fail Running the test from the Agilent Lab Monitor amp Diagnostic Software 1 Select the pressure test from the test selection menu 2 Start the test and follow the instructions Evaluating the Results on page 100 describes the evaluation and interpretation of the pressure test results For detailed instructions refer to the Agilent Lab Monitor amp Diagnostic Software Tool 1200 Series Capillary Pump User Manual 99 6 Troubleshooting and Diagnostics Evaluating the Results The sum of all leaks between the pump and the blank nut will be indicated by a pressure drop of gt 2 bar minute at the plateau Note that small leaks may cause the test to fail but solvent may not be seen leaking from a module Please notice the difference between an error in the test and a failure of the test An error means that during the operation of the test there was an abnormal termination If a test failed this means that the results of the test where not within the specified limits Often it is only a damaged blank nut itself poorly shaped from overtightening that causes a failure of the test Before investigating on any other possible sources of failure make sure that the blank nut you are using is in good condition and properly tightened 100 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Leak Test Capillary Pump Leak Test Description The leak test is a built in troubleshooting test designed to
64. he volume previously sucked into chamber 1 Because of the 2 1 speed ratio of the pistons half of the solvent flow from chamber 1 is forced out of the pump head continuing into the pump hydraulic path The other half of the flow from chamber 1 simultaneously refills chamber 2 When piston 1 has completed its delivery stroke the pistons reverse direction and the cycle is repeated gt To mixing chamber Seal Piston Ball screw drive Gear Motor with encoder Figure 3 Operating Principle of the Pump Head 1200 Series Capillary Pump User Manual 13 1 14 Introduction to the Capillary Pump Table 1 Capillary Pump Details continued Materials in contact with mobile phase Pump head SST gold sapphire ceramic Active Inlet Valve SST gold sapphire ruby ceramic PTFE Outlet Valve SST gold sapphire ruby tantalum Adapter SST gold EMPV SST ruby sapphire PEEK Flow Sensor SST Damping Unit Gold SST Capillaries Fused Silica For pump specifications see Site Requirements on page 24 1200 Series Capillary Pump User Manual Introduction to the Capillary Pump 1 How Does Compressibility Compensation Work The compressibility of the solvents in use will affect retention time stability when the back pressure in the system changes for example aging of column In order to minimize this effect the pump provides a compressibility compensation feature which optimizes the flow stabil
65. hexagonal key 4 mm hexagonal key Parts required Part number 1 5063 6586 Description Plunger Maintenance 7 1 Disassemble the pump head assembly see Removing and Disassembling the Pump Head Assembly on page 134 1200 Series Capillary Pump User Manual 2 Check the plunger surface and remove any deposits or layers Cleaning can be done with alcohol or tooth paste Replace plunger if scratched P Plunger surface 139 7 Maintenance Simple Repair Procedures 3 Reassemble the pump head assembly see Reassembling the Pump Head Assembly on page 142 140 1200 Series Capillary Pump User Manual Maintenance 7 Exchanging the Flow Sensor When Extended flow range 100 ul needed Leak on the flow sensor Unstable column flow Flow sensor blocked Tools required Screwdriver Pozidriv 1 Parts required Part number Description 1 Flow Sensor G1376 60001 20ul G1376 60002 100 ul 1 Turn off the pump 2 Using a 1 4 inch wrench disconnect the capillaries coming from the EMPV going to the injection device port 1 3 Unscrew the flow sensor 4 Re install the new one 5 Using a 1 4 inch wrench reconnect the capillaries coming from the EMPV going to the injection device port 1 1200 Series Capillary Pump User Manual 141 7 Maintenance Reassembling the Pump Head Assembly Tools required 3 mm hexagonal key 4 mm hexagonal key PTFE lubricant 79841 65501
66. hich are user selectable 1200 Series Capillary Pump User Manual Introduction to the Capillary Pump 1 Early Maintenance Feedback EMF The early maintenance feedback EMF feature monitors the usage of specific components in the instrument and provides feedback when the user settable limits have been exceeded The visual feedback in the user interface provides an indication that maintenance procedures should be scheduled For details on EMF counters and how to use them see Agilent Lab Advisor 1200 Series Capillary Pump User Manual 17 1 Introduction to the Capillary Pump Instrument Layout 18 The industrial design of the module incorporates several innovative features It uses Agilent s E PAC concept for the packaging of electronics and mechanical assemblies This concept is based upon the use of expanded polypropylene EPP layers foam plastic spacers in which the mechanical and electronic boards components of the module are placed This pack is then housed in a metal inner cabinet which is enclosed by a plastic external cabinet The advantages of this packaging technology are e virtual elimination of fixing screws bolts or ties reducing the number of components and increasing the speed of assembly disassembly e the plastic layers have air channels molded into them so that cooling air can be guided exactly to the required locations e the plastic layers help cushion the electronic and mechanical parts from physical
67. hould always be performed when the EMPV is suspected of being leaky or contaminated with particles 1200 Series Capillary Pump User Manual 71 6 Troubleshooting and Diagnostics Status Indicators Two status indicators are located on the front of the capillary pump The lower left one indicates the power supply status the upper right one indicates the instrument status Status indicator Power supply indicator Figure 12 Location of Status Indicators Power Supply Indicator The power supply indicator is integrated into the main power switch When the indicator is illuminated green the power is ON When the indicator is off the module is turned OFF Otherwhise check power connections availability of power or check functioning of the power supply 72 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Instrument Status Indicator The instrument status indicator indicates one of four possible instrument conditions When the status indicator is OFF and power switch light is on the capillary pump is in a prerun condition and is ready to begin an analysis A green status indicator indicates the capillary pump is performing an analysis run mode A yellow indicator indicates a not ready condition The capillary pump is in a not ready state when it is waiting for a specific condition to be reached or completed for example immediately after changing a setpoint or while a sel
68. ic Path Overview 10 How Does the Pumping Unit Work 12 How Does Compressibility Compensation Work 15 How Does Variable Stroke Volume Work 15 Early Maintenance Feedback EMF 17 Instrument Layout 18 The Electronics 19 Electrical Connections 20 Agilent 1200 Series Interfaces 22 ee Agilent Technologies 1 Introduction to the Capillary Pump Introduction to the Capillary Pump The capillary pump consists of two identical pumping units in a single housing It generates gradients by high pressure mixing A solvent selection valve provides flexibility in the choice of solvents The capillary pump is a binary pump Mobile phase composition is produced by mixing the outputs of pump A and pump B The solvent selection valve allows the pump A output to originate from either channel Al or channel A2 The pump B output may originate from either channel B1 or channel B2 Solvent degassing is not done directly in the pump A 4 channel low volume vacuum degasser available as a separate module provides degassed solvents to the pump channel inputs Solvent degassing is required for best flow stability and detector stability especially at the low flow rates required to run capillary LC applications 8 1200 Series Capillary Pump User Manual Introduction to the Capillary Pump 1 Introduction to the Capillary Pump Power supply CSM board Pump drive Damper Mixer Outlet valve Pump head A Flow sensor Active inlet valve Pump head B
69. iew 35 stack configuration rearview 36 stack configuration 34 status indicators 72 status indicators 70 stroke volume 15 stroke length 93 T temperature limit exceeded 86 temperature out of range 86 temperature sensor 77 timeout 75 190 tools screwdriver pozidriv 1 136 screwdriver pozidriv 1 132 wrench 1 4 inch 136 U unpacking the pump 32 V variable stroke volume 15 voltage range 20 27 voltage selector 20 WwW wait timeout 94 wash seals 123 141 waste tube 33 waste electrical and electronic equipment 180 WEEE directive 180 weight 27 wrench 1 4inch 99 103 130 136 wrench 14mm 126 127 128 130 wrench 1 4inch 134 wrench 1 4 5 16inch 33 wrench 14mm 33 Z zero solvent counter 81 1200 Series Capillary Pump User Manual Index 191 1200 Series Capillary Pump User Manual www agilent com In This Book This manual contains technical reference information about the Agilent 1200 Series capillary pump The manual describes the following e introduction to the pump e requirements and specifications e installation e using the pump e optimizing performance e troubleshooting and diagnostics e maintenance e parts and materials e overview of cables e legal safety and warranty information Agilent Technologies 2007 2008 Printed in Germany 11 08 G1376 90012 fe Agilent Technologies
70. ilent 1100 1200 to 3396A Integrators Connector03394 60600 Pin 3394 Pin Agilent Signal Name Active 1100 1200 TTL es 9 1 White Digital ground NC 2 Brown Prepare run Low 80 A 3 3 Gray Start Low bs NC 4 Blue Shut down Low ae o NC 5 Pink Not connected le NC 6 Yellow Power on High 5 14 7 Red Ready High 1 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected Agilent 1100 1200 to 3396 Series II 3395A Integrators Use the cable part number 03394 60600 and cut pin 5 on the integrator side Otherwise the integrator prints START not ready 1200 Series Capillary Pump User Manual 165 9 Identifying Cables Agilent 1100 1200 to 3396 Series III 3395B Integrators Connector03396 61010 Pin 33XX Pin Agilent Signal Name Active 1100 1200 TTL _ 9 1 White Digital ground NC 2 Brown Prepare run Low 8 3 3 Gray Start Low NC 4 Blue Shut down Low NC 5 Pink Not connected 1 NC 6 Yellow Power on High O 14 7 Red Ready High 4 8 Green Stop Low NC 9 Black Start request Low 13 15 Not connected Agilent 1100 1200 to HP 1050 HP 1046A or Agilent 35900 A D Converters Connector5061 3378 Pin HP Pin Agilent Signal Name Active 1050 1100 1200 TTL 1 White 1 White Digital ground 2 Brown 2 Brown Prepare run Low 3 Gray 3 Gray Start Low 4 Blue 4 Blue Shut down Low 5 Pin
71. imately 8 seconds Plateau 3 Plunger Al with a flow rate of 3 ul min for 30 seconds Ramp 6 Plunger B1 delivers 50 ul min for approximately 7 seconds Plateau 4 Plunger B1 delivers with a flow rate of 3 ul min for approximately 30 seconds At the end of the fourth plateau the test is finished and the capillary pump switches off 102 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Running the Leak Test When When problems with the capillary pump are suspected Tools required Wrench 1 4 inch Parts required Part number Description 1 G1313 87305 Restriction Capillary 1 01080 83202 Blank nut 500 ml lsopropanol Preparations Place two bottles of LC grade isopropyl alcohol in channels A2 and B2 Make absolutely sure that all parts of the flow path that are part of the test are very thoroughly flushed with IPA before starting to pressurize the system Any trace of other solvents or the smallest air bubble inside the flow path definitely will cause the test to fail Running the test from the Agilent Lab Monitor amp Diagnostic Software 1 Select the leak test from the test selection menu 2 Start the test and follow the instructions Make sure to release the pressure by slowly opening the purge valve when the test has finished Evaluating the Results on page 104 describes the evaluation and interpretation of the leak test results For detailed instructions refer to the Agilent Lab Monitor a
72. ing 65 Troubleshooting and Diagnostics 67 Agilent Lab Advisor Software 69 Overview of the Pump s Indicators and Test Functions 70 Status Indicators 72 User Interfaces 74 Error Messages 75 Micro Mode Pressure Test 95 Normal Mode Pressure Test 98 Leak Test 101 Flow Sensor Solvent Calibration 109 EMPV Test 112 EMPV Cleaning 113 Maintenance 115 Introduction to Maintenance and Repair 116 Early Maintenance Feedback EMF 119 Overview of Maintenance and Repair 121 Simple Repair Procedures 123 Parts and Materials for Maintenance 145 Pump Housing and Main Assemblies 146 Solvent Cabinet and Bottle Head Assembly 149 Hydraulic Path 150 Pump Head Assembly 152 Flow Sensor Assembly 154 Capillary Pump Accessory Kit 155 Identifying Cables 157 Cable Overview 158 Analog Cables 160 Remote Cables 163 BCD Cables 168 Auxiliary Cable 170 CAN LAN Cables 171 External Contact Cable 172 1200 Series Capillary Pump User Manual Contents RS 232 Cable Kit 173 10 Appendix 175 General Safety Information 176 The Waste Electrical and Electronic Equipment Directive 180 Lithium Batteries Information 181 Radio Interference 182 Sound Emission 183 Solvent Information 184 Agilent Technologies on Internet 186 1200 Series Capillary Pump User Manual Contents 6 1200 Series Capillary Pump User Manual 1200 Series Capillary Pump User Manual 1 Introduction to the Capillary Pump Introduction to the Capillary Pump 8 Hydraul
73. ing containers for any signs of damage If the containers or cushioning material are damaged save them until the contents have been checked for completeness and the instrument has been mechanically and electrically checked If the shipping container or cushioning material is damaged notify the carrier and save the shipping material for the carrier s inspection Delivery Checklist Ensure all parts and materials have been delivered with the capillary pump The delivery checklist is shown in Table 5 on page 32 To aid in parts identification please see Parts and Materials for Maintenance on page 145 Please report missing or damaged parts to your local Agilent Technologies sales and service office Table5 Capillary Pump Checklist Description Quantity Capillary pump 1 Solvent cabinet 1 5062 8591 Solvent bottle 1X9301 1450 amber bottle 3X9301 1420 transparent bottle Bottle head assembly 4 1367 60003 Capillary G1375 87310 Power cable 1 CAN cable 1 m 1 Remote cable As ordered Signal cable As ordered 1200 Series Capillary Pump User Manual Installing the Pump 3 Table5 Capillary Pump Checklist Description Quantity Service Manual 1 Accessory kit see Table 6 1 on page 33 Accessory Kit Contents Capillary Pump Table6 Accessory Kit Contents G1376 68705 Description Part Number Quantity Seal insert tool 01018 23702 1 Wrench 1 4 5 16 inch 8710 0510 1 Wrench 14 mm 8710 1924 1 Wrench 7 1
74. ing drive assembly a servo controlled variable reluctance motor and gear train assembly are used to move two ball screw drives The gear train moves the two ball screw drives in opposite directions 180 degree out of phase The gear ratios are designed such that the first ball screw drive constantly moves at twice the speed of the second ball screw drive The servo motor includes a high resolution shaft position encoder which continuously reports the speed and direction of the motor in real time This speed and direction information is used by the pump control electronics to ensure precise control of the servo motor movement Each pump head consists of two identical chambers pistons and seals plus an active inlet valve and an outlet ball valve The solvent volume in each chamber is displaced by its piston The pistons are directly moved by the reciprocating ball screw drives of the metering drive assembly Due to the gear design of the metering drive assembly the pistons move in opposite directions with piston 1 constantly moving at twice the speed of piston 2 The outer diameter of the piston is smaller than the inner diameter of the chamber allowing solvent to flow in the gap between the piston and the chamber wall The two chambers are connected by the pressure dependent outlet ball valve The position of the solvent selection valve determines which of two solvents will be sucked low pressure through the active inlet valve into chamber 1
75. ite and initiate appropriate actions 1 Place the Pump horizontally on the bench 1200 Series Capillary Pump User Manual 37 3 Installing the Pump Installing the Capillary Pump 2 Ensure the power switch on the front of the capillary pump is OFF switch stands out Status Lamp Power Switch Serial number Figure 7 Front of Capillary Pump 3 At the rear of the module move the security lever to its maximum right position 4 Connect the power cable to the power connector at the rear of the module The security lever will prevent that the cover is opened while the power cord is connected to the module 38 1200 Series Capillary Pump User Manual Installing the Pump 3 Installing the Capillary Pump 5 Connect the required interface cables to the rear of the capillary pump see Connecting Agilent 1200 Series modules on page 40 Configuration switch GPIB _ _ tt sid Slot for interface board E E RS232 Remote Analog output CAN Bus Power Plug Security Lever Figure 8 Rear of Capillary Pump 6 Connect the capillary solvent tubes and waste tubings see Flow Connections of the Capillary Pump on page 42 7 Press the power switch to turn the pump on NOTE The power switch stays pressed in and the green indicator LED in the power switch is on while the pump is turned on When the line power switch stands out and the green light is off the pump is turned off
76. ity according to the solvent type The compressibility compensation is set to a default value for each pump head independently The compensation value for each pump head can be changed through the user interface Without a compressibility compensation the following will happen during a stroke of the first piston The pressure in the piston chamber increases and the volume in the chamber will be compressed depending on backpressure and solvent type The volume displaced into the system will be reduced by the compressed volume When a compressibility compensation value for a pump head is set the pump processor calculates a compensation volume that depends on the system pressure and the selected compressibility value This compensation volume is added to the delivery stroke of the first piston How Does Variable Stroke Volume Work Due to the compression of the pump chamber volume each piston stroke of the pump will generate a small pressure pulsation influencing the flow ripple of the pump The amplitude of the pressure pulsation is mainly dependent on the stroke volume and the compressibility compensation for the solvent in use Small stroke volumes will generate less pressure pulsations than higher stroke volumes at same flow rates In addition the frequency of the pressure pulsations will be higher This will decrease the influence of flow pulsations on quantitative results In gradient mode smaller stroke volumes resulting in less flow ripp
77. ive Action Loose or leaky fitting Tighten the fitting or exchange the capillary Untight EMPV Run the EMPV test Damaged pump seals or plungers Run the leak test to confirm the leak High flow sensor offset Run the flow sensor accuracy calibration and correct the flow sensor offset Potential Cause Autosampler Corrective Action Loose or leaky fitting Tighten or exchange the fitting or capillary Needle seat Exchange the needle seat Rotor seal injection valve Exchange the rotor seal Damaged metering seal or plunger Exchange the metering seal Check the plunger for scratches Exchange the plunger if required 1200 Series Capillary Pump User Manual 97 6 Troubleshooting and Diagnostics Normal Mode Pressure Test 98 Capillary Pump Normal Mode Pressure Test The pressure test is a quick built in test designed to demonstrate the pressure tightness of the system The test involves monitoring the pressure profile as the capillary pump runs through a predefined pumping sequence The resulting pressure profile provides information about the pressure tightness of the system Step 1 The test begins with the initialization of both pumpheads After initialization plungers Al and B1 are both at the top of their stroke Next pump A begins pumping solvent with a flow rate of 510 ul min and stroke of 100 ul The capillary pump continues to pump until a system pressure of 390 bar is reached For this test only chann
78. k 5 Pink Not connected 6 Yellow 6 Yellow Power on High 7 Red 7 Red Ready High 8 Green 8 Green Stop Low 9 Black 9 Black Start request Low 166 1200 Series Capillary Pump User Manual Agilent 1100 1200 to HP 1090 LC or Signal Distribution Module Identifying Cables 9 Connector01046 60202 Pin HP 1090 Pin Agilent Signal Name Active 1100 1200 TTL 1 1 White Digital ground NC 2 Brown Prepare run Low 7 4 3 Gray Start Low E A a E 7 4 Blue Shut down Low si 8 5 Pink Not connected l NC 6 Yellow Power on High 3 7 Red Ready High 6 8 Green Stop Low NC 9 Black Start request Low Agilent 1100 1200 to General Purpose Connector01046 60201 Pin Universal Pin Agilent Signal Name Active 1100 1200 TTL 1 White Digital ground i l 2 Brown Prepare run Low DE KEY 3 Gray Start Low m i a 4 Blue Shut down Low ss oo 5 Pink Not connected i 7 6 Yellow Power on High 7 Red Ready High 8 Green Stop Low 9 Black Start request Low 1200 Series Capillary Pump User Manual 167 9 Identifying Cables BCD Cables a 000600000 A Oleaceovo One end of these cables provides a 15 pin BCD connector to be connected to the Agilent 1200 Series modules The other end depends on the instrument to be connected to Agilent 1200 to General Purpose Connector G1351 81600 Wir
79. le will improve composition ripple The capillary pump uses a processor controlled ball screw system to drive its pistons The normal stroke volume is optimized for the selected flow rate Small flow rates use a small stroke volume while higher flow rates use a higher stroke volume 1200 Series Capillary Pump User Manual 15 1 16 Introduction to the Capillary Pump The stroke volume for the pump is set to AUTO mode This means that the stroke is optimized for the flow rate in use A change to larger stroke volumes is possible but not recommended When the pump is in the standard mode the EMPV is fully closed Total main flow up to 2500 ul min is directed to the LC system Column flow measurement control is disabled This mode is for non capillary LC applications In the capillary mode the standard flow sensor measures and controls column flow in the range of 0 01 ul min to 20 ul min An extended range flow sensor optional provides flow measurement and control in the range of 0 01 ul min to 100 ul min Flow measurement is based on the principle of mass flow temperature sensitivity The flow sensor consists of a heated tube with two temperature sensors As the mobile phase passes through the heated tube the temperature characteristic distributed over the two temperature sensors is evaluated From the temperature characteristic flow rate accuracy is determined The flow sensor measurement is calibrated for specific mobile phases w
80. lectrical Connections 20 The GPIB connector is used to connect the capillary pump with a computer The address and control switch module next to the GPIB connector determines the GPIB address of your capillary pump The switches are preset to a default address which is recognized once after power on The CAN bus is a serial bus with high speed data transfer The two connectors for the CAN bus are used for internal Agilent 1200 Series module data transfer and synchronization One analog output provides a signal for integrators or data handling systems The REMOTE connector may be used in combination with other analytical instruments from Agilent Technologies if you want to use features such as common shut down prepare and so on The RS 232 connector may be used to control the capillary pump from a computer via RS 232 connection using appropriate software This connector needs to be activated by the configuration switch module next to the GPIB connector The software needs the appropriate drivers to support this communication See your software documentation for further information The power input socket accepts a line voltage of 100 240 volts AC 10 with a line frequency of 50 or 60 Hz Maximum power consumption is 220 VA Volt Amps There is no voltage selector on your capillary pump because the power supply has wide ranging capability There are no externally accessible fuses because automatic electronic fuses are implemen
81. lent Lab Advisor Software 69 Overview of the Pump s Indicators and Test Functions 70 Status Indicators 70 Error Messages 70 Pressure Test 70 Leak Test 70 Flow Sensor Calibration 71 EMPV Test 71 EMPV Cleaning 71 Status Indicators 72 Power Supply Indicator 72 Instrument Status Indicator 73 User Interfaces 74 Error Messages 75 Micro Mode Pressure Test 95 Description 95 Running the Test from the Agilent Lab Monitor amp Diagnostic Software 96 Micro Mode Pressure Test Results 97 Normal Mode Pressure Test 98 Capillary Pump Normal Mode Pressure Test 98 Running the Pressure Test 99 Evaluating the Results 100 Leak Test 101 Capillary Pump Leak Test Description 101 Running the Leak Test 103 Evaluating the Results 104 ait Agilent Technologies 67 6 68 Troubleshooting and Diagnostics Flow Sensor Solvent Calibration 109 Description 109 Running the Calibration Routine 110 EMPV Test 112 EMPV Test Description 112 Running the EMPV Test 112 EMPV Cleaning 113 Capillary Pump EMPV Cleaning Description 113 Running the Test 113 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Agilent Lab Advisor Software The Agilent Lab Advisor Software is a standalone product that can be used with or without data system Agilent Lab Advisor helps to manage the lab for high quality chromatographic results and can monitor in real time a single Agilent LC or all the Agilent GCs and LCs configured on the lab intran
82. ll nitric acid some capillary columns can be damaged by nitric acid 3 Replace the filter 1200 Series Capillary Pump User Manual 125 7 Maintenance Exchanging the Active Inlet Valve Cartridge or the Active Inlet Valve Removing the Active Inlet Valve When If internally leaking backflow Tools required Wrench 14 mm Parts required Part number Description 1 G1312 60025 Active inlet valve body 1 5062 8562 Valve cartridge 400 bar 1 Unplug the active inlet valve cable from the connector 2 Disconnect the solvent inlet tube at the inlet valve beware of leaking solvents 3 Using a 14 mm wrench loosen the active inlet valve and remove the valve from pump head Active inlet valve body Valve cartridge Figure 15 Active Inlet Valve Parts 126 1200 Series Capillary Pump User Manual When Tools required Parts required Maintenance Exchanging the Valve Cartridge If internally leaking backflow Wrench 14 mm Part number Description 1 G1312 60025 Active inlet valve body 1 5062 8562 Valve cartridge 400 bar 1 Using a pair of tweezers remove the valve cartridge from the actuator assembly 2 Before inserting the new valve cartridge clean the area in the actuator assembly Fill a syringe with alcohol and flush the cartridge area thoroughly 3 Insert a new valve cartridge into the actuator assembly make sure the valve cartridge is fully inserted into the actuator assembly 1200 Series Capillary Pump
83. logies 115 7 Maintenance Introduction to Maintenance and Repair Simple Repairs Maintenance The capillary pump is designed for easy repair The most frequent repairs such as plunger seal change and filter frit change can be done with the capillary pump in place in the system stack These repairs are described in Table 11 on page 123 Exchanging Internal Parts Some repairs may require exchange of defective internal parts Exchange of these parts requires removing the module from the stack removing the covers and disassembling the module The security lever at the power input socket prevents that the module cover is taken off when line power is still connected 116 1200 Series Capillary Pump User Manual Maintenance 7 Warnings and Cautions Module is partially energized when switched off as long as the power cord is plugged in Risk of stroke and other personal injury Repair work at the module can lead to personal injuries e g shock hazard when the module cover is opened and the instrument is connected to power gt Never perform any adjustment maintenance or repair of the module with the top cover removed and with the power cord plugged in gt The security lever at the power input socket prevents that the module cover is taken off when line power is still connected Never plug the power line back in when cover is removed When opening capillary or tube fittings solvents may leak out The handling of toxic a
84. luding springs G1311 60002 3 Support ring 5001 3739 4 Seal pack of 2 or 5063 6589 Seal pack of 2 for normal phase applications 0905 1420 5 Capillary outlet valve to piston 2 G1312 67300 6 Pump chamber housing G1311 25200 7 Active inlet valve without cartridge G1312 60025 Replacement cartridge for active inlet valve 5062 8562 8 Outlet ball valve G1312 60012 9 Screw lock 5042 1303 10 Apdater G1312 23201 11 Screw M5 60 mm lg 0515 2118 152 1200 Series Capillary Pump User Manual Parts and Materials for Maintenance 8 Pump Head Assembly Figure 25 Pump Head Assembly 1200 Series Capillary Pump User Manual 153 8 Parts and Materials for Maintenance Flow Sensor Assembly Table 17 Flow Sensor Assembly Item Description Part Number 1 Flow sensor assembly 20 pl G1376 60001 Flow sensor assembly 100 pl G1376 60002 Capillary EMPV to flow sensor 20 ul flow sensor G1375 87301 Capillary EMPV to flow sensor 100 pl flow sensor G1375 87305 Capillary flow sensor to injection device 20 pl flow sensor G1375 87310 Capillary flow sensor to injection device 100 pl flow sensor G1375 87306 Figure 26 Flow Sensor Assembly 154 1200 Series Capillary Pump User Manual Parts and Materials for Maintenance 8 Capillary Pump Accessory Kit Table 18 Accessory Kit G1376 68705 Description Part Number Tubing flexible 2 m 0890 1760 SST Frit 2 um Oty 1 5022 2185 Wrench open end 7 16 1 2 inch Oty
85. ly A blocked solvent filter in the bottle especially when only partly blocked is more difficult to identify and may show up as gradient performance problems intermittent pressure fluctuations etc Algae growth may also be the possible source for failures of the ball valves and other components in the flow path How to Prevent and or Reduce the Algae Problem Always use freshly prepared solvents especially use demineralized water which was filtered through about 0 2 um filters Never leave mobile phase in the instrument for several days without flow Always discard old mobile phase Use the amber solvent bottle part number 9301 1450 supplied with the instrument for your aqueous mobile phase If possible add a few mg l sodium azide or a few percent organic solvent to the aqueous mobile phase 1200 Series Capillary Pump User Manual 55 4 Using the Capillary Pump Inject the Check out Sample 56 The purpose of the instrument check is to demonstrate that all modules of the instrument are correctly installed and connected It is not a test of the instrument performance A single injection of the Agilent Technologies isocratic test standard is made under the conditions given below Conditions Table 7 Conditions Flow 15 0 pl minute Stoptime 7 00 minutes Solvent A 30 HPLC grade Water Solvent B 70 HPLC grade Acetonitrile Wavelength DAD MWD Sample 254 4 nm Reference 360 80 nm Injector Volume
86. mp Diagnostic Software Tool 1200 Series Capillary Pump User Manual 103 6 Troubleshooting and Diagnostics Evaluating the Results Defective or leaky components in the pump head lead to changes in the leak test pressure plot Typical failure modes are described below Please notice the difference between an error in the test and a failure of the test An error means that during the operation of the test there was an abnormal termination If a test failed this means that the results of the test where not within the specified limits Often it is only a damaged blank nut itself poorly shaped from overtightening that causes a failure of the test Before investigating on any other possible sources of failure make sure that the blank nut you are using is in good condition and properly tightened No pressure increase or minimum pressure of plateau 1 not reached Probable cause Suggested actions 1 Pump not running Check the logbook for error messages 2 Wrong solvent line connections to solvent Ensure the solvent lines from the degasser to selection valve the solvent selection valve are connected correctly 3 Loose or leaky fittings Ensure all fittings are tight or exchange capillary 4 Large leaks visible at the pump seals Exchange the pump seals 5 Large leaks visible at active inlet valve Ensure the leaky components are installed outlet valve or EMPV tightly Exchange the component if required Run the EMPV cleaning pr
87. n an external instrument with a remote connection to the system 3 Shut down in an external instrument with a remote connection to the system 4 The degasser failed to generate sufficient vacuum for solvent degassing Remote Timeout Suggested actions Fix the leak in the external instrument before restarting the module Fix the leak in the external instrument before restarting the module Check external instruments for a shut down condition Check the vacuum degasser for an error condition Refer to the Service Manual for the Agilent 1200 Series vacuum degasser A not ready condition is still present on the remote input When an analysis is started the system expects all not ready conditions e g a not ready condition during detector balance to switch to run conditions within one minute of starting the analysis If a not ready condition is still present on the remote line after one minute the error message is generated Probable cause 1 Not ready condition in one of the instruments connected to the remote line 2 Defective remote cable 3 Defective components in the instrument showing the not ready condition Suggested actions Ensure the instrument showing the not ready condition is installed correctly and is set up correctly for analysis Exchange the remote cable Check the instrument for defects refer to the instrument s reference documentation 1200 Series Capillary Pump User Manual Synchroniza
88. n and display through instant pilot and maintenance Agilent Lab Monitor amp Diagnostic Software leak detection safe leak handling leak output signal for shutdown of pumping system Low voltages in major maintenance areas GLP features Early maintenance feedback EMF for continuous tracking of instrument usage in terms of seal wear and volume of pumped mobile phase with user settable limits and feedback messages Electronic records of maintenance and errors Housing All materials recyclable 1200 Series Capillary Pump User Manual 29 2 Site Requirements and Specifications Performance Specifications 30 1200 Series Capillary Pump User Manual 1200 Series Capillary Pump User Manual 3 Installing the Pump Unpacking the Capillary Pump 32 Damaged Packaging 32 Delivery Checklist 32 Accessory Kit Contents Capillary Pump 33 Optimizing the Stack Configuration 34 Installing the Capillary Pump 37 3 Installing the Pump 31 Connecting Modules and Control Software 40 40 Connecting Agilent 1200 Series modules Connecting an Agilent 1200 Series Vacuum Degasser Connecting control software and or control modules Flow Connections of the Capillary Pump 42 46 Get the System Ready for the First Injection Priming your capillary LC system with the pump 46 40 41 ka a Agilent Technologies 31 3 Installing the Pump Unpacking the Capillary Pump 32 Damaged Packaging Upon receipt of your module inspect the shipp
89. nd the blank nut is measured 1200 Series Capillary Pump User Manual 95 6 Troubleshooting and Diagnostics Running the Test from the Agilent Lab Monitor amp Diagnostic Software 1 Select the Micro Mode Pressure Test from the test selection menu 2 Start the test and follow the instructions For detailed instructions refer to the Agilent Lab Monitor amp Diagnostic Software In step 10 of following procedure if you block the flow sensor outlet use the PEEK blank nut provided in the accessory kit Don t connect a SST blank nut to the flow sensor outlet this could damage the flow sensor 96 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Micro Mode Pressure Test Results The test results are evaluated automatically The sum of all leaks within the column flow path from the EMPV to the blank nut must be lower than 1000 nl min Small leaks with no visible leaks in the flow path can cause the test to fail If the pressure test fails Ensure all fittings between the pump and the blank nut are tight and repeat the pressure test If the test fails again insert the blank nut at the outlet of the previous module in the stack and repeat the pressure test Exclude each module one by one to determine which module is leaky Potential Causes of Pressure Test Failure After isolating and fixing the cause of the leak repeat the pressure test to confirm the system is tight Potential Cause Pump Correct
90. nd hazardous solvents and reagents can hold health risks gt Please observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the solvent vendor especially when toxic or hazardous solvents are used CAUTION Electronic boards are static sensitive and should be handled with care so as not to damage them Touching electronic boards and components can cause electrostatic discharge ESD ESD can damage electronic boards and components gt Be sure to hold the board by the edges and do not touch the electrical components Always use an ESD protection for example an ESD wrist strap when handling electronic boards and components 1200 Series Capillary Pump User Manual 117 7 Maintenance Using the ESD Strap 1 Unwrap the first two folds of the band and wrap the exposed adhesive side firmly around your wrist 2 Unroll the rest of the band and peel the liner from the copper foil at the opposite end 3 Attach the copper foil to a convenient and exposed electrical ground Figure 13 Using the ESD Strap Cleaning the Module Liquid dripping into the electronic compartment of your module Liquid in the module electronics can cause shock hazard and damage the module gt Do not use an exessively damp cloth during cleaning gt Drain all solvent lines before opening any fittings The module case should be ke
91. nd require a different seal when used for a longer time in the pump For applications that use normal phase solvents for example hexane we recommend the use of the polyethylene seals part number 0905 1420 pack of 2 These seals have less abrasion compared to the standard seals Polyethylene seals have a limited pressure range 0 200 bar When used above 200 bar their lifetime will be significantly reduced DO NOT apply the seal wear in procedure performed with new standard seals at 400 bar 1200 Series Capillary Pump User Manual 61 5 Optimizing Performance How to Choose the Primary Flow The primary flow can be sets in three ranges e The default range The default range is the best compromise between performance and solvent consumption e The low solvent consumption range The low solvent consumption range is recommended for long shallow gradient runs e g peptide maps It is not privileged when the application requires fast gradient The selection of this range can result in less performance e The fast gradient range This range is recommended for running fast gradient e g lt 3 min The equilibration time is optimized The primary flow is strongly dependant on the system pressure and the configuration of the pump namely which filter flow sensor and mixer are installed in the pump Table 8 on page 62 gives approximate primary flow values in function of the system pressure and the set primary flow range Ta
92. nlet port of the solvent selection valve or the adapter at the active inlet valve When opening capillary or tube fittings solvents may leak out The handling of toxic and hazardous solvents and reagents can hold health risks gt Please observe appropriate safety procedures for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the solvent vendor especially when toxic or hazardous solvents are used CAUTION Small particles can permanently block the capillaries and valves of the module Damage of the module gt Always filter solvents gt Never use the module without solvent inlet filter 124 The solvent filters are located on the low pressure side of the capillary pump A blocked filter therefore does not affect the pressure readings of the capillary pump The pressure readings cannot be used to check whether the filter is blocked or not If the filter is in good condition the solvent will freely drip out of the solvent tube due to hydrostatic pressure If the solvent filter is partly blocked only very little solvent will drip out of the solvent tube 1200 Series Capillary Pump User Manual Maintenance 7 Cleaning the Solvent Filters 1 Remove the blocked solvent filter from the bottle head assembly and place it in a beaker with concentrated nitric acid 35 for one hour 2 Thoroughly flush the filter with bidistilled water remove a
93. nnected to Agilent 1100 1200 to 3390 Integrators Connector 01046 60203 Pin 3390 Pin Agilent Signal Name Active 1100 1200 TTL 2 1 White Digital ground NC 2 Brown Prepare run Low 7 3 Gray Start Low a NC 4 Blue Shut down Low NC 5 Pink Not connected NC 6 Yellow Power on High NC 7 Red Ready High NC 8 Green Stop Low NC 9 Black Start request Low 1200 Series Capillary Pump User Manual 163 9 Identifying Cables Agilent 1100 1200 to 3392 3 Integrators Connector01046 60206 Pin 3392 3 Pin Agilent Signal Name Active 1100 1200 TTL 3 1 White Digital ground NC 2 Brown Prepare run Low 11 3 Gray Start Low NC 4 Blue Shut down Low NC 5 Pink Not connected NC 6 Yellow Power on High 9 7 Red Ready High 1 8 Green Stop Low NC 9 Black Start request Low Agilent 1100 1200 to 3394 Integrators Connector01046 60210 Pin 3394 Pin Agilent Signal Name Active 1100 1200 TTL 9 1 White Digital ground NC 2 Brown Prepare run Low 80 15 s 3 3 Gray Start Low NC 4 Blue Shut down Low e o NC 5 Pink Not connected 16 zi NC 6 Yellow Power on High O 5 14 7 Red Ready High 6 8 Green Stop Low 1 9 Black Start request Low 13 15 Not connected 164 1200 Series Capillary Pump User Manual Identifying Cables 9 START and STOP are connected via diodes to pin 3 of the 3394 connector Ag
94. nnection cable Exchange the solvent selection valve 83 84 Troubleshooting and Diagnostics Missing Pressure Reading The pressure readings read by the pump ADC analog digital converter are missing The ADC reads the pressure readings from the damper every Ims If the readings are missing for longer than 10 seconds the error message is generated Probable cause Suggested actions 1 Damper not connected Ensure the damper is connected clean and seated correctly 2 Defective damper Exchange the damper 3 Defective main board Exchange the main board Pump Configuration At switch on the pump has recognized a new pump configuration The pump is assigned its configuration at the factory If the active inlet valve and pump encoder of channel B are disconnected and the pump is rebooted the error message is generated However the pump will function as an isocratic pump in this configuration The error message reappears after each switch on Probable cause Suggested actions 1 Active inlet valve and pump encoder of Reconnect the active inlet valve and pump channel B disconnected encoder of channel B 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Valve Fuse Valve Fuse 0 Channels Al and A2 Valve Fuse 1 Channels B1 and B2 One of the solvent selection valves in the pump has drawn excessive current causing the selection valve electronic fuse to open Probable cause Suggested actions
95. nnel you must ensure the miscibility of the solvent that no precipitation of buffer occurs Plug the pump outlet with blank nut at EMPV outlet Disconnect the EMPV to flow sensor at the EMPV outlet Plug the EMPV outlet port with blank nut 01080 83202 Execute test Check result with Pressure Test if necessary Remove the blank nut Reconnect the EMPV to flow sensor capillary Do not overtighten 1200 Series Capillary Pump User Manual 113 6 Troubleshooting and Diagnostics EMPV Cleaning 114 1200 Series Capillary Pump User Manual 1200 Series Capillary Pump User Manual 7 Maintenance Introduction to Maintenance and Repair 116 Simple Repairs Maintenance 116 Exchanging Internal Parts 116 Warnings and Cautions 117 Using the ESD Strap 118 Cleaning the Module 118 Early Maintenance Feedback EMF 119 EMF Counters 119 Using the EMF Counters 120 Overview of Maintenance and Repair 121 Simple Repair Procedures 123 Checking and Cleaning the Solvent Inlet Filters 124 Exchanging the Active Inlet Valve Cartridge or the Active Inlet Valve 126 Exchanging the Outlet Ball Valve Sieve or the Complete Valve 130 Exchanging the Solvent Selection Valve 132 Removing and Disassembling the Pump Head Assembly 134 Exchanging the Pump Seals and Seal Wear in Procedure 136 Exchanging the Plungers 139 Exchanging the Flow Sensor 141 Reassembling the Pump Head Assembly 142 Exchanging the Optional Interface Board 144 ott Agilent Techno
96. nstrument and protective covers removed Energy available at many points may if contacted result in personal injury Any adjustment maintenance and repair of the opened instrument under voltage should be avoided whenever possible When inevitable this has to be carried out by a skilled person who is aware of the hazard involved Do not attempt internal service or adjustment unless another person capable of rendering first aid and resuscitation is present Do not replace components with power cable connected Do not operate the instrument in the presence of flammable gases or fumes Operation of any electrical instrument in such an environment constitutes a definite safety hazard Do not install substitute parts or make any unauthorized modification to the instrument Capacitors inside the instrument may still be charged even though the instrument has been disconnected from its source of supply Dangerous voltages capable of causing serious personal injury are present in this instrument Use extreme caution when handling testing and adjusting 1200 Series Capillary Pump User Manual 177 10 Appendix When working with solvents please observe appropriate safety procedures e g goggles safety gloves and protective clothing as described in the material handling and safety data sheet by the solvent vendor especially when toxic or hazardous solvents are used 178 1200 Series Capillary Pump User Manual Appendix 10 Safety Symb
97. nt 1100 1200 Series modules The other end depends on the instrument to which connection is being made Agilent 1100 1200 to 3390 2 3 Integrators Connector 01040 60101 Pin 3390 2 3 Pin Agilent Signal Name 1100 1200 1 Shield Ground 2 Not connected 8 7 3 Center Signal 6 F F REN 4 Connected to pin 6 S Al 5 Shield Analog ME 6 Connected to pin 4 7 Key 8 Not connected 160 1200 Series Capillary Pump User Manual Identifying Cables 9 Agilent 1100 1200 to 3394 6 Integrators Connector35900 60750 Pin 3394 6 Pin Agilent Signal Name 1100 1200 1 Not connected 2 Shield Analog 3 Center Analog GIN 000 Agilent 1100 1200 to BNC Connector Connector8120 1840 Pin BNC Pin Agilent Signal Name 1100 1200 leq aS Shield Shield Analog HO Center Center Analog et 1200 Series Capillary Pump User Manual 161 9 Identifying Cables Agilent 1100 1200 to General Purpose Connector01046 60105 Pin 3394 6 Pin Agilent Signal Name 1100 1200 1 Not connected 2 Black Analog a 3 Red Analog 162 1200 Series Capillary Pump User Manual Remote Cables Identifying Cables 9 One end of these cables provides a Agilent Technologies APG Analytical Products Group remote connector to be connected to Agilent 1100 1200 Series modules The other end depends on the instrument to be co
98. ocedure 104 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Pressure limit not reached but plateaus horizontal or positive Probable cause 1 Degasser and pump channels A and or B not flushed sufficiently air in the channels 2 Wrong solvent All plateaus negative Probable cause 1 Loose or leaky fittings 2 Leaky mixer if installed 3 Contaminated EMPV 4 Loose pump head screws in channel A or B 5 Leaking seal or scratched plunger in channel A2 or B2 6 Leaking outlet valve in channel A or B 7 Leaky damper 1200 Series Capillary Pump User Manual Suggested actions Purge the degasser and pump channels thoroughly with isopropanol under pressure use the restriction capillary Install isopropanol Purge the degasser and pump channels thoroughly Suggested actions Ensure all fittings are tight or exchange capillary Tighten the mixer fittings and nuts Run the EMPV cleaning procedure Ensure the pump head screws in channels A and B are tight Exchange the pump seals in both channels Check the plungers for scratches Exchange if scratched Exchange the outlet valve Exchange damper 105 6 106 Troubleshooting and Diagnostics First plateau negative or unstable and at least one other plateau positive Probable cause 1 Leaking outlet valve in channel A 2 Loose pump head screws in channel A 3 Leaking seal or scratched plunger in channel
99. of a leak Purge the module Run a pressure test to determine whether the seals or other module components are defective Exchange the damper Exchange the main board 1200 Series Capillary Pump User Manual Pressure Signal Missing Troubleshooting and Diagnostics 6 The pressure signal from the damper is missing The pressure signal from the damper must be within a specific voltage range If the pressure signal is missing the processor detects a voltage of approximately 120mV across the damper connector Probable cause 1 Damper disconnected 2 Defective damper Valve Failed Valve 0 Failed valve A1 Valve 1 Failed valve A2 Valve 2 Failed valve B2 Valve 3 Failed valve B1 Suggested actions Ensure the damper is connected correctly to the main board Exchange the damper One of the solvent selection valves in the module failed to switch correctly The processor monitors the valve voltage before and after each switching cycle If the voltages are outside expected limits the error message is generated Probable cause 1 Solvent selection valve disconnected 2 Connection cable inside instrument not connected 3 Connection cable inside instrument defective 4 Solvent selection valve defective 1200 Series Capillary Pump User Manual Suggested actions Ensure the solvent selection valve is connected correctly Ensure the connection cable is connected correctly Exchange the co
100. ols Table 19 Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to the instruction manual in order to protect risk of harm to the operator and to protect the apparatus against damage Indicates dangerous voltages Indicates a protected ground terminal Indicates eye damage may result from directly viewing the light produced by the deuterium lamp used in this product The apparatus is marked with this symbol when hot surfaces are available and the user should not touch it when heated up A WARNING alerts you to situations that could cause physical injury or death gt Do not proceed beyond a warning until you have fully understood and met the indicated conditions CAUTION A CAUTION alerts you to situations that could cause loss of data or damage of equipment gt Do not proceed beyond a caution until you have fully understood and met the indicated conditions 1200 Series Capillary Pump User Manual 179 10 Appendix The Waste Electrical and Electronic Equipment Directive Abstract The Waste Electrical and Electronic Equipment WEEE Directive 2002 96 EC adopted by EU Commission on 13 February 2003 is introducing producer responsibility on all electric and electronic appliances starting with 13 August 2005 This product complies with the WEEE Directive 2002 96 EC marking requirements The affixed label indicates that you must not discard
101. ools required Wrench 1 4 inch Wrench 14 mm Parts required Part number Description 1 G1312 60008 Outlet ball valve 1 5063 6505 Sieve pack of 10 Before exchanging the outlet ball valve you can try to clean it in a sonic bath Remove the gold seal and the sieve Place the valve in upright position onto the plastic cap in a small beaker with alcohol Place in a sonic bath for 5 to 10 minutes Insert a new sieve and replace the gold seal 1 Using a 1 4 inch wrench disconnect the valve capillary from the outlet ball valve 2 Using the 14 mm wrench loosen the valve and remove it from the pump body 3 Remove the plastic cap with the gold seal from the outlet ball valve 4 Using a pair of tweezers remove the sieve Check the gold seal It should be exchanged when strongly deformed Place the valve in an upright position insert the sieve into the recess and replace the gold seal with the cap Make sure that the sieve cannot move and is away from the seal area of the gold seal 5 Place a new sieve into the recess of the outlet ball valve and replace the cap with the gold seal 130 1200 Series Capillary Pump User Manual Maintenance 7 Simple Repair Procedures 6 Check that the new valve is assembled correctly and that the gold seal is present Valve body Sieve Gold seal Plastic cap Figure 17 Outlet Ball Valve Parts 7 Reinstall the outlet ball valve and tighten the valve 8 Reconnect the valve capillary V
102. oth liquimeters can be assigned an EMF maximum limit When the limit is exceeded the EMF flag in the user interface is displayed 1200 Series Capillary Pump User Manual 119 7 120 Maintenance Seal Wear Counters The seal wear counters display a value derived from pressure and flow both contribute to seal wear The values increment with pump usage until the counters are reset after seal maintenance Both seal wear counters can be assigned an EMF maximum limit When the limit is exceeded the EMF flag in the user interface is displayed Using the EMF Counters The user settable EMF limits for the EMF counters enable the early maintenance feedback to be adapted to specific user requirements The wear of pump components is dependent on the analytical conditions therefore the definition of the maximum limits need to be determined based on the specific operating conditions of the instrument Setting the EMF Limits The setting of the EMF limits must be optimized over one or two maintenance cycles Initially no EMF limit should be set When performance indicates maintenance is necessary take note of the values displayed by pump liquimeter and seal wear counters Enter these values or values slightly less than the displayed values as EMF limits and then reset the EMF counters to zero The next time the EMF counters exceed the new EMF limits the EMF flag will be displayed providing a reminder that maintenance needs to be sched
103. ousing parts 146 pump seals 123 136 purge valve 123 132 radio interference 182 reassembling the pump head 142 1200 Series Capillary Pump User Manual recommended pH range 28 remote connector 20 remote timeout 76 remote cable 158 163 removing the pump head 134 repair procedures 123 repairs using the ESD strap 118 restart without cover 81 results pressure test 100 RS 232C connector 20 RS 232 cable 159 RS 232C cable kitto PC 173 running the leak test 103 running the pressure test 99 S safety class 176 safety information lithium batteries 181 safety general information 176 176 standards 27 symbols 179 screwdriver pozidriv 1 136 141 screwdriver pozidriv 1 132 seal insert tool 33 seal wear counters 120 seal wear counter 137 seal alternative material 61 seals 123 139 security lever 38 116 selection valve failed 83 selection valve fuse 85 servo restart failed 90 189 Index setable flowrange 28 shipping containers 32 shut down 76 sieve 123 130 simple repair procedures 123 site requirements power considerations 25 snap fastener 42 solvent cabinet parts 149 solvent cabinet 43 50 solvent filters cleaning 125 solvent inlet filter 50 solvent bottle 32 solvent cabinet 32 solvent filters prevent blocking 53 solvent information 50 52 184 solvents 184 sonic bath 130 sound emission 183 sovent selection valve 132 specification performance 28 physical 27 stack configuration front v
104. pared to the standard one Never run the capillary pump without an inline filter 64 1200 Series Capillary Pump User Manual Optimizing Performance 5 How to Optimize the Compressibility Compensation Setting The compressibility compensation default settings are 50 x 10 bar best for most aqueous solutions for pump head A and 115 x 106 bar to suit organic solvents for pump head B The settings represent average values for aqueous solvents A side and organic solvents B side Therefore it is always recommended to use the aqueous solvent on the A side of the pump and the organic solvent on the B side Under normal conditions the default settings reduce the pressure pulsation to values below 1 of system pressure that will be sufficient for most applications If the compressibility values for the solvents used differ from the default settings it is recommended to change the compressibility values accordingly Compressibility settings can be optimized by using the values for various solvents described in Table 9 on page 66 If the solvent in use is not listed in the compressibility table when using premixed solvents and if the default settings are not sufficient for your application the following procedure can be used to optimize the compressibility settings Use the capillary pump in the Normal Mode at least 100 pl min 1 Start channel A of the capillary pump with the adequate flow rate The system pressure must be between 50 and 25
105. pt clean Cleaning should be done with a soft cloth slightly dampened with water or a solution of water and a mild detergent Do not use an excessively damp cloth that liquid can drip into the module 118 1200 Series Capillary Pump User Manual Maintenance 7 Early Maintenance Feedback EMF Maintenance requires the exchange of components in the flow path which are subject to mechanical wear or stress Ideally the frequency at which components are exchanged should be based on the intensity of usage of the instrument and the analytical conditions and not on a predefined time interval The early maintenance feedback EMF feature monitors the usage of specific components in the instrument and provides feedback when the user settable limits have been exceeded The visual feedback in the user interface provides an indication that maintenance procedures should be scheduled EMF Counters The pump provides a series of EMF counters for the pump head Each counter increments with pump use and can be assigned a maximum limit which provides visual feedback in the user interface when the limit is exceeded Each counter can be reset to zero after maintenance has been done The pump provides the following EMF counters e liquimeter pump A e seal wear pump A e liquimeter pump B e seal wear pump B Liquimeters The liquimeters display the total volume of solvent pumped by the left and right pump heads since the last reset of the counters B
106. r this 1200 Series Capillary Pump User Manual 51 4 Using the Capillary Pump Solvent Information Always filter solvents through 0 4 um filters small particles can permanently block the capillaries and valves Avoid the use of the following steel corrosive solvents 52 Solutions of alkali halides and their respective acids for example lithium iodide potassium chloride and so on High concentrations of inorganic acids like sulfuric and nitric acid especially at higher temperatures replace if your chromatography method allows by phosphoric acid or phosphate buffer which are less corrosive against stainless steel Halogenated solvents or mixtures which form radicals and or acids for example 2CHCly O gt gt 2COCl 2HC1 This reaction in which stainless steel probably acts as a catalyst occurs quickly with dried chloroform if the drying process removes the stabilizing alcohol Chromatographic grade ethers which can contain peroxides for example THF dioxane di isopropylether Such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides Solvents containing strong complexing agents e g EDTA Mixtures of carbon tetrachloride with 2 propanol or THF dissolve stainless steel Avoid the use of alkaline solutions pH gt 8 5 which can attack the fused silica from the capillaries 1200 Series Capillary Pump User Manual Using the Capillary Pump 4 Prevent Blocking of Solven
107. rms in the sep arate agreement shall control Technology Licenses The hardware and or software described in this document are furnished under a license and may be used or copied only in accor dance with the terms of such license Restricted Rights Legend If software is for use in the performance of a U S Government prime contract or subcon tract Software is delivered and licensed as Commercial computer software as defined in DFAR 252 227 7014 June 1995 or as a commercial item as defined in FAR 2 101 a or as Restricted computer soft ware as defined in FAR 52 227 19 June 1987 or any equivalent agency regulation or contract clause Use duplication or dis closure of Software is subject to Agilent Technologies standard commercial license terms and non DOD Departments and Agencies of the U S Government will receive no greater than Restricted Rights as defined in FAR 52 227 19 c 1 2 June 1987 U S Government users will receive no greater than Limited Rights as defined in FAR 52 227 14 June 1987 or DFAR 252 227 7015 b 2 November 1995 as applicable in any technical data Safety Notices CAUTION A CAUTION notice denotes a hazard It calls attention to an operating procedure practice or the like that if not correctly per formed or adhered to could result in damage to the product or loss of important data Do not proceed beyond a CAUTION notice until the indicated condi tions ar
108. s for example goggles safety gloves and protective clothing as described in the material handling and safety data sheet supplied by the solvent vendor especially when toxic or hazardous solvents are used At the pump activate the Purge Mode and set the flow rate to 2 5 ml min 2 Flush the vacuum degasser and all tubes with at least 5 ml of solvent 3 Set flow to required value of your application and activate the pump micro mode 4 Pump for approximately 5 minutes before starting your application 5 Repeat step 1 on page 46 through step 2 on page 46 for the other channel s of the capillary pump 46 1200 Series Capillary Pump User Manual Installing the Pump 3 When the pumping system has been turned off for a certain time for example overnight oxygen will re diffuse into the solvent channel between the vacuum degasser and the pump Solvents containing volatile ingredients will slightly lose these if left in the degasser without flow for a prolonged period of time Therefore purging each channel at 2 5 ml min for 1 minute is required before starting an application 1200 Series Capillary Pump User Manual 47 3 48 Installing the Pump Get the System Ready for the First Injection 1200 Series Capillary Pump User Manual 1200 Series Capillary Pump User Manual 4 Using the Capillary Pump Hints for Successful Use of the Capillary Pump 50 Solvent Information 52 Prevent Blocking of Solvent Filters 53 Algae Growth in
109. s suspected of being inaccurate or the desired solvent combination is not listed in the predefined calibration table Salts and small amounts of organic modifiers don t have a significant influence on the calibration data In this cases the pre defined aqueous curves can be used Check the flow sensor accuracy at the upper flow rate with water A system with inaccurate calibration data will still produce reproducible results Before starting the calibration routine the pump must pass the leak test The routine is set up to calibrate unknown solvents in channel Al and B1 of the solvent selection valve First the system is equilibrated with pure water from channel A2 At 15 ul min the system switches to pressure control and keeps the pressure constant for the procedure A step to 100 A1 is done results response of the aqueous phase relative to water and then a step gradient from 0 A1 to 100 B1 results response of unknown mixtures Solvents e Al Aqueous solvent to be calibrated 1200 Series Capillary Pump User Manual 109 6 110 Troubleshooting and Diagnostics e B1 Organic solvent to be calibrated e A2 Pure water reference solvent Running the Calibration Routine 1 Fill vacuum degasser with appropriate solvents and purge each channel at 2500 ul min for 3 minutes Remove the capillary at the flow sensor outlet Check that the standard flow sensor is installed 20 ul flow sensor Disconnect the
110. sor short 78 hexagonal key 3mm 136 139 142 hexagonal key 3mm 134 leak sensor open 78 leak test evaluation 104 1200 Series Capillary Pump User Manual Index leak test 101 leak test 70 leak 77 line frequency 20 27 line voltage 20 27 liquimeter 137 lithium batteries 181 M main assemblies parts 146 main assemblies overview 121 maintenance procedures 119 maintenance procedures 17 message ignition without cover 80 80 issing pressure reading 84 issing parts 32 3 3 3 otor drive power 87 non operating altitude 27 non operating temperature 27 0 operating Altitude 27 operating temperature 27 optimum performance 34 outlet ball valve 130 outlet ball valve 123 overview pump 10 P parts main assemblies 146 parts accessory kit 155 bottle head assembly 149 damaged 32 flow sensor 154 hydraulic path 150 missing 32 pump head 152 pump housing 146 solvent cabinet 149 performance specification 28 pH range 28 physical specifications 27 piston 123 139 power supply indicator 72 power supply lamp 72 power switch 38 power consumption 27 power cords 24 power considerations 25 pressure above upper limit 82 pressure below lower limit 82 pressure pulsation 15 pressure sensor readings 41 pressure pulsation 65 pressure range 61 pressure test 70 pressure operating range 28 priming witha pump 46 PTFE lubricant 142 PTFE frit 123 132 pump head assembly 152 pump head missing 91 pump h
111. st of the mobile phase mixing is accomplished The mixer output flow called main flow is connected to the Electronic Flow Control EFC system The EFC system consists of an Electro Magnetic Proportioning Valve EMPV in series with a Flow Sensor The EMPV is protected from particles in the mobile phase by a solvent filter frit Responding to user entered column flow setpoint the EFC system determines how much of the main flow volume is ultimately delivered to the column The remaining main flow volume which is not required by the column is diverted to waste by the EMPV Under user control the EMPV can also function as a purge valve for purposes of solvent changeover etc In this case the EMPV is totally open and the total main flow is diverted to waste 1200 Series Capillary Pump User Manual Introduction to the Capillary Pump 1 Introduction to the Capillary Pump From solvent bottle Pump head B Piston Seal Inlet Mixing Outlet ale chamber Valve I Inlet Outlet valve valve Flow sensor Damper Filter To waste Figure2 The Hydraulic Path 1200 Series Capillary Pump User Manual 11 1 12 Introduction to the Capillary Pump How Does the Pumping Unit Work Both pumping units channel A and channel B are identical with respect to parts and function Each pumping unit consists of a pump head which is directly attached to a metering drive assembly In each meter
112. t Filters Contaminated solvents or algae growth in the solvent bottle will reduce the lifetime of the solvent filter and will influence the performance of the module This is especially true for aqueous solvents or phosphate buffers pH 4 to 7 The following suggestions will prolong lifetime of the solvent filter and will maintain the performance of the module e Use a sterile if possible amber solvent bottle to slow down algae growth e Filter solvents through filters or membranes that remove algae e Exchange solvents every two days or refilter e If the application permits add 0 0001 0 001M sodium azide to the solvent e Place a layer of argon on top of your solvent e Avoid exposure of the solvent bottle to direct sunlight Never use the system without solvent filter installed 1200 Series Capillary Pump User Manual 53 4 Using the Capillary Pump Algae Growth in HPLC Systems 54 The presence of algae in HPLC systems can cause a variety of problems that may be incorrectly diagnosed as instrument or application problems Algae grow in aqueous media preferably in a pH range of 4 8 Their growth is accelerated by buffers for example phosphate or acetate Since algae grow through photosynthesis light will also stimulate their growth Even in distilled water small sized algae grow after some time Instrumental Problems Associated With Algae Algae deposit and grow everywhere within the HPLC system causing e Deposits on b
113. t the APG cable to the APG remote connector of the pump see Figure 6 on page 36 5 Press in the power switches to turn on the vacuum degasser 40 1200 Series Capillary Pump User Manual Installing the Pump 3 The AUX output allows the user to monitor the vacuum level in the degasser chamber Connecting control software and or control modules 1 Ensure the power switches on the front of the modules in the stack are OFF switches stand out 2 Plug a GPIB cable into the GPIB connector at one of the modules preferably at the detector MUST for the DAD 3 Connect the GPIB cable to the Agilent control software in use 4 Plug a CAN cable into the CAN connector of the control module Do not connect the Agilent control software or the control module with the vacuum degasser 5 Connect the CAN cable to the CAN connector of one of the modules 6 Press in the power switches to turn on the modules The Agilent control software e g ChemStation EZChrom OL etc can be also be connected to the system through a LAN cable which requires the installation of a LAN board For more information about connecting the control module or Agilent control software refer to the respective user manual For connecting the Agilent 1200 Series equipment to non Agilent 1200 Series equipment see Introduction to the Capillary Pump on page 8 1200 Series Capillary Pump User Manual 41 3 Installing the Pump Flow Connections of the Capillary Pump
114. ted in the power supply The security lever at the power input socket prevents that the capillary pump cover is taken off when line power is still connected The interface board slot is used for BCD output LAN and for future use 1200 Series Capillary Pump User Manual Introduction to the Capillary Pump 1 Electrical Connections Configuration switch GPIB Slot for interface board RS232 Remote Analog output CAN Bus Power plug Security lever Figure 4 Electrical Connections to the Capillary Pump 1200 Series Capillary Pump User Manual 21 1 Introduction to the Capillary Pump Agilent 1200 Series Interfaces The Agilent 1200 Series modules provide the following interfaces Table 2 Agilent 1200 Series Interfaces Interface Type Pumps Autosampler DA Detector DA Detector VW Detector Thermostatted Vacuum MW Detector MW Detector RI Detector Column Degasser LC Detector G1315C Compartment G1365C CAN Yes Yes Yes Yes Yes Yes No LAN on board No No No Yes No No No GBIP Yes Yes Yes No Yes No No RS 232C Yes Yes Yes Yes Yes Yes No Remote Yes Yes Yes Yes Yes Yes Yes Analog Yes No 2x 2x 1x No Yes LAN BCD Ext Yes Yes Yes Yes Yes No No 1 The vacuum degasser will have a special connector for specific use For details see description of main board 2 Interface slot for specific interfacing external contacts BCD LAN and so on For details on the available interfaces see service manual 22 1200 Series Capill
115. the Active Inlet Valve on page 126 Exchanging the Outlet Ball Valve Sieve or the Complete Valve on page 130 Exchanging the Solvent Selection Valve on page 132 Exchanging the Solvent Selection Valve on page 132 Exchanging the Pump Seals and Seal Wear in Procedure on page 136 Exchanging the Plungers on page 139 Exchanging the Flow Sensor on page 141 If internally leaking If internally leaking Unstable column flow or system pressure Column flow and system pressure drops from time to time If pump performance indicates seal wear If scratched Extended flow range 100 ul needed Leak on the flow sensor Unstable column flow Flow sensor blocked Pressure ripple unstable run leak test for verification Pressure ripple unstable run leak test for verification A pressure drop of gt 10 bar across the frit 2 5 ml min H20 with purge open indicates blockage Leaks at lower pump head side unstable retention times pressure ripple unstable run leak test for verification Seal life time shorter than normally expected check plungers while changing the seals 1200 Series Capillary Pump User Manual 123 7 Maintenance Checking and Cleaning the Solvent Inlet Filters When Parts required Preparations If solvent filter is blocked Description Concentrated nitric acid 65 Bidistilled water 1 Beaker Remove the solvent inlet tube from the i
116. tic Software Pressure Test The pressure test is a quick test designed to determine the pressure tightness of the system After exchanging flow path components e g pump seals or injection seal use this test to verify the system is pressure tight up to 400 bar see Description on page 95 and Capillary Pump Normal Mode Pressure Test on page 98 Leak Test The leak test is a diagnostic test designed to determine the pressure tightness of the capillary pump When a problem with the capillary pump is suspected use this test to help troubleshoot the capillary pump and its pumping performance see Capillary Pump Leak Test Description on page 101 70 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Flow Sensor Calibration The flow sensor calibration procedure is designed to generate customized calibration data This procedure should be run whenever the flow rate is suspected of being inaccurate or the desired solvent combination is not listed in the predefined calibration table EMPV Test The EMPV test is designed to verify the performance of the EMPV This test must always be done when the EMPV valve is exchanged The test should also be done if column flow stability problems occur micro mode only EMPV Cleaning Depending on the application sometimes particles can be collected in the EMPV valve This cleaning procedure is designed to remove the particle deposits This procedure s
117. tion Lost Troubleshooting and Diagnostics 6 During an analysis the internal synchronization or communication between one or more of the modules in the system has failed The system processors continually monitor the system configuration If one or more of the modules is no longer recognized as being connected to the system the error message is generated Probable cause 1 CAN cable disconnected 2 Defective CAN cable 3 Defective main board in a different module Leak A leak was detected in the module Suggested actions Ensure all the CAN cables are connected correctly Ensure all CAN cables are installed correctly Exchange the CAN cable Switch off the system Restart the system and determine which module or modules are not recognized by the system The signals from the two temperature sensors leak sensor and board mounted temperature compensation sensor are used by the leak algorithm to determine whether a leak is present When a leak occurs the leak sensor is cooled by the solvent This changes the resistance of the leak sensor which is sensed by the leak sensor circuit on the main board Probable cause 1 Loose fittings 2 Broken capillary 3 Loose or leaking active inlet valve outlet ball valve or EMPV 4 Defective pump seals 1200 Series Capillary Pump User Manual Suggested actions Ensure all fittings are tight Exchange defective capillaries Ensure pump components are seated corre
118. ugated waste tube to the waste outlet of the pump leak handling system Purge your system before first use see Priming your capillary LC system with the pump on page 46 1200 Series Capillary Pump User Manual 43 3 Installing the Pump Flow Connections of the Capillary Pump To port 1 of the injection valve Waste Pump head A Pump head B Figure 10 Flow connection of the capillary pump G1375 87301 01090 87308 01090 87308 A wo N G1375 87400 1200 Series Capillary Pump User Manual Installing the Pump 3 Flow Connections of the Capillary Pump 5 G1375 87310 6 G1312 67304 7 G1312 67302 8 G1311 67304 9 G1311 60003 1200 Series Capillary Pump User Manual 45 3 Installing the Pump Get the System Ready for the First Injection When you are using the system for the first time it is recommended to prime it to remove all the air and the possible contamination introduced in the flow path during the installation The pump should never be used for priming empty tubings never let the pump run dry Use the syringe to draw enough solvent for completely filling the tubings to the pump inlet before continuing to prime with the pump Priming your capillary LC system with the pump WARNING When opening capillary or tube fittings solvents may leak out The handling of toxic and hazardous solvents and reagents can hold health risks gt Please observe appropriate safety procedure
119. uled 1200 Series Capillary Pump User Manual Maintenance 7 Overview of Maintenance and Repair Overview of Maintenance and Repair Figure 14 on page 121 shows the main assemblies of the capillary pump The pump heads and its parts do require normal maintenance for example seal exchange and can be accessed from the front simple repairs Replacing internal parts will require to remove the module from its stack and to open the top cover 5 6 7 4 3 8 9 10 2 11 12 1 Figure 14 Overview of Repair Procedures 1 Leak sensor see service manual 2 Active inlet valve see Removing the Active Inlet Valve on page 126 3 Outlet ball valve see Exchanging the Outlet Ball Valve Sieve or the Complete Valve on page 130 1200 Series Capillary Pump User Manual 121 7 Maintenance 4 EMPV see service manual 5 Pump drive see service manual 6 Power supply see service manual 7 CSM board see service manual 8 Fan see service manual 9 Damper see service manual 10 Flow sensor see Exchanging the Flow Sensor on page 141 11 not installed 12 Solvent selection valve see Exchanging the Solvent Selection Valve on page 132 122 1200 Series Capillary Pump User Manual Simple Repair Procedures Maintenance 7 The procedures described in this section can be done with the capillary pump in place in the system stack Table 11 Simple Repair Procedures Procedure Symptom Notes Removing
120. ump User Manual Troubleshooting and Diagnostics 6 Error Messages Error messages are displayed in the user interface when an electronic mechanical or hydraulic flow path failure occurs which requires attention before the analysis can be continued for example repair frit exchange or exchange of consumables required In the event of such a failure the red status indicator at the front of the module is switched on and an entry is written into the instrument logbook Timeout The timeout threshold was exceeded Probable cause Suggested actions 1 The analysis was completed successfully Check the logbook for the occurrence and and the timeout function switched off the source of a not ready condition Restart the module as requested analysis where required 2 Anot ready condition was present duringa Check the logbook for the occurrence and sequence or multiple injection run for a source of a not ready condition Restart the period longer than the timeout threshold analysis where required 1200 Series Capillary Pump User Manual 75 76 Troubleshooting and Diagnostics Shut Down An external instrument has generated a shut down signal on the remote line The module continually monitors the remote input connectors for status signals A LOW signal input on pin 4 of the remote connector generates the error message Probable cause 1 Leak detected in another module with a CAN connection to the system 2 Leak detected i
121. ump has wide ranging capabilities and accepts any line voltage in the range mentioned in Table 3 on page 27 Consequently there is no voltage selector at the back of the instrument There are also no externally accessible fuses as automatic electronic fuses are implemented in the power supply Module is partially energized when switched off as long as the power cord is plugged in Repair work at the module can lead to personal injuries e g shock hazard when the cover is opened and the module is connected to power gt Make sure that it is always possible to access the power plug gt Remove the power cable from the instrument before opening the cover gt Do not connect the power cable to the Instrument while the covers are removed Incorrect line voltage at the instrument Shock hazard or damage of your instrumentation can result if the devices are connected to a line voltage higher than specified gt Connect your instrument to the specified line voltage CAUTION Unaccessable power plug In case of emergency it must be possible to disconnect the instrument from the power line at any time gt Make sure the power connector of the instrument can be easily reached and unplugged gt Provide sufficient space behind the power socket of the instrument to unplug the cable 1200 Series Capillary Pump User Manual 25 2 Site Requirements and Specifications Bench Space The module dimensions and weight see
122. ve in channel A 14mm wrench Do not overtighten Ensure the pump head screws in channel A are tight Ensure the sieve in the outlet valve is installed correctly Tighten the outlet valve Exchange the pump seals in channel A Check the plungers for scratches Exchange if scratched Exchange the active inlet valve in channel A 107 6 6 Troubleshooting and Diagnostics Fourth plateau negative or unstable and at least one other plateau positive Probable cause Suggested actions 1 Airin pump chamber of channel B or seals Flush channel B thoroughly with isopropanol not yet seated under pressure restriction capillary 2 Loose active inlet valve in channel B Tighten the active inlet valve in channel B 14mm wrench Do not overtighten 3 Loose pump head screws in channel B Ensure the pump head screws in channel B are tight 4 Loose outlet valve in channel B Ensure the sieve in the outlet valve is installed correctly Tighten the outlet valve 5 Leaking seal or scratched plunger in channel Exchange the pump seals in channel B Check B1 the plungers for scratches Exchange if scratched 6 Defective active inlet valve in channel B Exchange the active inlet valve in channel B 108 1200 Series Capillary Pump User Manual Troubleshooting and Diagnostics 6 Flow Sensor Solvent Calibration Description This routine is designed to generate customized calibration data The routine should be run whenever the flow rate i

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