Waters HPLC Installation And Maintenance Manual Download

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Waters Prep Series

Installation and Maintenance Guide

71500045204/Revision

Summary of Contents for HPLC

Page 2: ...errors that may appear in this document This document is believed to be complete and accurate at the time of publication In no event shall Waters Corporation be liable for incidental or consequential...

Page 3: ...disposal of any Waters product You can reach us via the Internet telephone or conventional mail Safety considerations Some reagents and samples used with Waters instruments and devices can pose chemi...

Page 4: ...nted in this section Applicable symbols Audience and purpose This guide is intended for personnel who install and maintain the Waters Prep Series HPLC system Symbol Definition Manufacturer location Au...

Page 5: ...for calibration instructions Quality control Routinely run three QC samples that represent subnormal normal and above normal levels of a compound Ensure that QC sample results fall within an acceptab...

Page 6: ...vi EC authorized representative Waters Corporation Micromass UK Ltd Floats Road Wythenshawe Manchester M23 9LZ United Kingdom Telephone 44 161 946 2400 Fax 44 161 946 2480 Contact Quality manager...

Page 7: ...rep Series HPLC system v Calibrating v Quality control v ISM classification v ISM Classification ISM Group 1 Class B v EC authorized representative vi 1 Overview 1 1 Waters Prep series 1 2 PrepLC syst...

Page 8: ...ine connections 2 21 Connecting a helium tank to the fluid handling unit 2 30 Helium specifications 2 30 Sparging 2 31 Connecting compression fittings 2 31 Setting up the plunger wash 2 33 Considerati...

Page 9: ...charts 3 5 Chromatography troubleshooting 3 16 Hardware troubleshooting 3 23 Software troubleshooting 3 31 Performance tests 3 36 Self diagnostics 3 36 Extended tests 3 37 Maintenance procedures 3 47...

Page 10: ...C 1 D Solvent Considerations D 1 Clean solvent D 2 Solvent miscibility D 3 How to use miscibility numbers M numbers D 5 Buffered solvents D 6 Solvent head height D 6 Solvent viscosity D 6 Solvent deg...

Page 11: ...HPLC systems in two configurations Waters PrepLC System Waters Delta Prep System Tip Although the two systems share many features certain aspects nevertheless differ This guide addresses both differe...

Page 12: ...ou access previously created gradient event and detector tables Preprogrammed gradient profiles System control of external PowerLine detectors and autoinjectors is through an IEEE 488 interface RS 232...

Page 13: ...000 L volume heads The 500 L pump heads permit flow rates of 1 to 150 mL min and the 1000 L heads permit flow rates of 4 to 300 mL min The system allows easy scale up so you need not replumb to change...

Page 14: ...vices Fluid handling unit Contains components for delivering solvents from their reservoirs to the injector or column It consists of the pump and plunger wash pump solvent sparge valve assembly and so...

Page 15: ...In the small scale system the injector is in a flow path plumbed with 0 009 inch ID tubing In the large scale system solvent flows from the pump to the large scale injector through 0 040 inch ID tubin...

Page 16: ...ning valve They then flow to the pump inlet manifold where the flow path branches at two inlet check valves The pump heads draw solvent through the valves moving 500 and 1000 L with each stroke with a...

Page 17: ...ver the controller is on circulating solvent by pushing a small volume along the flow path one pulse per minute PrepLC controller The figure below shows the Waters PrepLC controller which controls sol...

Page 18: ...are The controller s OPERATE METHOD screen allows direct control of the switches Program control is through the time based PROGRAM EVENT screen where you must specify each switch as ON OFF or PULSE Ti...

Page 19: ...cations interface The inject start terminal becomes an output when you forgo using an injector in favor of starting the run with screen keys Thus the inject start terminal synchronizes controller oper...

Page 20: ...expecting contact closures If the controlled input is polarized connect the grounds together and the input terminal to the Hold output Analog Output Press Chart Special output produces a DC voltage wh...

Page 21: ...ly cord It also provides for selecting operating voltage Auxiliary power fuse Contains a 1 5 A fuse for the 12 VAC accessory power terminal Pump power fuse Contains a 4 A fuse 5 20 mm Connecting cable...

Page 22: ...hrough the purge valve and continues to the mixer From there it goes to the Rheodyne 7725i injector the analytical column the small scale outlet port and the detector Large scale flow path When you se...

Page 23: ...ters Prep Series You can program the fraction collector itself for maximum flexibility and productivity SE 120 chart recorder The SE 120 is a two pen recorder that can simultaneously plot two analog s...

Page 24: ...ncludes an RI reference flush valve Accessories such as autoinjectors or detectors are available from your Waters sales representative Getting started This section describes using the Waters Prep Seri...

Page 25: ...e mode The self diagnostics test each PowerLine module in the Waters Prep Series These modules include Controller and pump Detectors e g Waters 2487 or 2414 Autoinjector Waters 717plus If all tests ru...

Page 26: ...l as messages from the system It also shows the cursor a bright rectangle against a dark background Controller keys The controller has three types of keys Keypad Cursor movement keys ENTER key CLEAR k...

Page 27: ...e press the HELP screen key 3 Press ENTER The program evaluates the new entry for proper type and range 4 An acceptable entry becomes the current parameter value and the cursor moves to the next logic...

Page 28: ...the screen label changes to display an alternate function For example when you press LOCK KEYBOARD the screen label changes to UNLOCK KEYBOARD The screen key labels might also indicate system status...

Page 29: ...fter cleaning the lines of any salts flush the system with Milli Q HPLC grade water containing at least 10 methanol Remove the column if it is incompatible with this storage protocol Flush the plunger...

Page 30: ...rs Waters 746 Data Module Automatically sets up and controls all gradient injection external event and detector parameters directly from the keyboard Uses a Method table that links time based control...

Page 31: ...perational steps to change wavelength and attenuation during a run You can create a Method table a time based program that can include up to 48 individual steps Each step accesses a set of Gradient Ev...

Page 32: ...oes not communicate with any PowerLine modules Nevertheless it can operate with any Waters data system or integrator connected to the IEEE or RS 232 ports Operation The Gradient controller stores 15 s...

Page 33: ...e back to itself to repeat a method Screen layout The figure below illustrates the layout of screens for the system s Gradient controller configuration Gradient controller screens See the Waters Prep...

Page 34: ...1 24 Overview...

Page 35: ...uirements 2 5 Assembling the system 2 7 Connecting a helium tank to the fluid handling unit 2 30 Setting up the plunger wash 2 33 Installing sample injection options 2 40 Connecting a fraction collect...

Page 36: ...n four cartons which together contain the following PrepLC controller electronics unit Fluid handling unit and Startup Kit Shelf unit Delta Prep system rack with column clamps and injector valves Acce...

Page 37: ...le connections Vibration is negligible The shelf unit rests securely on the bench The mixer in the PrepLC system has to be mounted vertical with the flow direction from bottom inlet to top outlet Delt...

Page 38: ...ers Delta Prep system dimensions on page 2 4 Tip Before installing the controller determine whether you must reconfigure the operating frequency and or operating voltage selections as outlined in Elec...

Page 39: ...s installed Voltage selections You can adapt the system to operate at the nominal voltages shown in the table below Changing the voltage The system is preset for 120 VAC operation To change the voltag...

Page 40: ...tage setting 6 Waters ships all controllers with 4 A fuses for 110 120 VAC operation If you operate the unit with 220 240 VAC change the fuse see step 7 If you do not need to change the fuse proceed t...

Page 41: ...The Rheodyne injector generates a signal output as it injects the sample Connect the cable for this output to the Inject terminal on the controller s rear panel Tip Cable polarity is irrelevant PrepLC...

Page 42: ...5i injectors to the controller connect the leads from the inject signal cable at the rear of the column rack to the Inject and Gnd terminals Injector connections to the controller Injector electrical...

Page 43: ...n the controller s rear panel If you are not using the M 1000 PrepPak module see Connecting additional devices on page 2 9 Stop flow connection from the optional M 1000 PrepPak module Connecting addit...

Page 44: ...the proportioning valve which differs from its composition inside the column or detector cell Plotting 1 Connect the leads at one end of the event cable Startup Kit to the Chart and Chart terminals 2...

Page 45: ...ections to the integrator or chart recorder on page 2 10 2 Connect the leads at the other end of the cable to the corresponding terminals for the second pen on the integrator or recorder External devi...

Page 46: ...evice 2 Connect the positive lead to the 12 VAC terminal on the controller and the negative lead to an available switch S1 to S4 terminal Tip The maximum current available from the 12 VAC power source...

Page 47: ...ting a fraction collector on page 2 42 To connect PowerLine detectors Waters 2487 and 2414 see IEEE 488 cables with external PowerLine devices on page 2 17 To connect detectors other than PowerLine de...

Page 48: ...see the figure Pump interface cable and power cord locations on page 2 14 3 Connect the other end of the 37 pin interface cable to the rear of the pump Pump interface cable and power cord locations Ca...

Page 49: ...the IEEE 488 startup sequence IEEE 488 cables with data systems When you control the Prep system from a Waters data system MassLynx or Empower workstations use the IEEE 488 interface to receive infor...

Page 50: ...er 717plus Autosampler 2487 Detector busLAC E card Empower or GPIB card MassLynx IEEE 488 connector IEEE 488 cable Data system PrepLC controller as gradient controller PrepLC controller as gradient co...

Page 51: ...nger tightness 6 Specify a unique IEEE 488 address from 2 to 29 for each device connected on the IEEE 488 bus see Setting IEEE 488 addresses on page 2 18 Perform the correct IEEE 488 startup sequence...

Page 52: ...mp Configuration screen When using the controller as a PowerLine controller you do not set the IEEE 488 address of the Prep system pump In the PowerLine system configuration set the IEEE 488 address f...

Page 53: ...ent controlled through the busLAC E module SAT IN modules and connected analog detectors 3 Start the pump establishing eluent flow Then start all other devices controlled through the IEEE 488 bus Tip...

Page 54: ...module Tip The interface transmits no chromatographic data Connecting the RS 232 To connect the RS 232 1 Connect the 25 pin connector provided with the data module to the rear panel of the data module...

Page 55: ...ittings as this section describes Do not nick kink or sharply bend the tubing This can restrict flow Tip Repeated bending of tubing causes tubing to fail Subjecting the system to a wide temperature fl...

Page 56: ...and 0 019 inch ID Fluid pathways Refer to the following illustrations when plumbing your Prep system The figure below shows tubing sizes for the standard PrepLC system s fluid pathways This system is...

Page 57: ...LC system fluid pathway The figure Delta Prep system fluid pathway on page 2 24 shows the fluid pathway in the Delta Prep system Large scale injector Purge outlet PrepLC pump Plunger seal wash pump Pl...

Page 58: ...ect the components Allow slack 2 Use a cutting file to circumscribe the tube at the point you want to cut it 3 Hold the tubing on either side of the scribe mark with two cloth covered pliers and gentl...

Page 59: ...ition Tip Subsequent connections to this fitting will not require the extra 3 4 turn Cutting PTFE tubing To cut PTFE tubing 1 Estimate or measure the length of tubing required to connect the component...

Page 60: ...n screw compresses the ferrule fusing it onto the tubing in the proper position Fluid handling unit connections This section describes these connections to the fluid handling unit Solvent reservoir se...

Page 61: ...a convenient location preferably at the same level as the fluid handling unit 2 Remove protective wrapping from these nine PTFE tubes Solvent A Solvent B Solvent C and Solvent D Sparge A Sparge B Spar...

Page 62: ...at preparative flow rates To connect a solvent reservoir to the fluid handling unit 1 Push a labeled solvent tube through a hole in the cap of a correspondingly labeled reservoir Tip Push tubing far...

Page 63: ...at higher flow rates can starve the pump of solvent The inlet tube s sharp edge can pare material from the inside the filter creating particles that can be sucked into the inlet line These particles...

Page 64: ...t includes the shutoff valve tubing and other fittings for connecting the sparge inlet to a 50 to 90 psi helium supply Helium sparging reduces the total dissolved gas in the solvent reservoirs and mai...

Page 65: ...e helium equilibrates at the gas liquid interface The displaced gases are carried to the surface and then expelled through the reservoir vent Tip For more information on this process see Appendix D Co...

Page 66: ...on the type of source fittings 2 Regulate the helium supply source to between 50 and 90 psi 3 5 and 6 3 atm 3 Connect the supply line from the helium source to the sparge fitting on the fluid handling...

Page 67: ...ricates the plunger reducing its wear and flushing away any mobile phase forced past its seal from the high pressure side of the pump head Caution You must set up the plunger wash when you initially i...

Page 68: ...h pump s inlet tubing into a reservoir containing a solvent that is compatible with your mobile phase Plunger wash connections 2 Connect outlet tubing to the wash fitting at the top of the left pump h...

Page 69: ...nnect the pump outlet to the injection panel 1 Cut a length of tubing to extend from the pump outlet to the unused fitting on the injector panel s purge valve or that goes directly to the column inlet...

Page 70: ...ckpressure Tip Waters offers optional small scale injector and scale select valves for the PrepLC system Contact your local Waters Technical Service representative for details Connecting a prep column...

Page 71: ...ep system The 0 040 inch ID and 0 009 inch ID tubing inside the Delta Prep system s column rack permit large and small scale operation The scale switching valve isolates one tubing pathway from the ot...

Page 72: ...20 Detector inlet Column outlet large scale Stainless 0 040 Detector inlet Recycle to pump PTFE 0 040 Recycle port on manual sample inlet valve Inlet from detector Stainless 0 040 Detector outlet TP01...

Page 73: ...ainless steel tubing Startup Kit that reaches from the pump outlet to the Inlet connector on the column rack s front panel Tip Use excess tubing forming it into several coils as shown in the figure Pu...

Page 74: ...scale sample injection valve option PrepLC system If you expect to routinely inject sample volumes of less than 2 mL volume Waters recommends you use the small scale manual injector valve option kit T...

Page 75: ...2 12 Connect column s to either valve as appropriate Using an autoinjector Tip Consult documentation provided with the autoinjector for complete information on this product Making electrical connecti...

Page 76: ...minal on the fraction collector to the controller To make the remote start connection 1 Connect the fraction collector s pin 3 to any vacant Gnd terminal on the controller 2 Connect the fraction colle...

Page 77: ...pLC system includes clamps and clamp holders for mounting a column vertically onto the shelf unit The figure below illustrates how to attach a preparative column Attaching the column Installing the co...

Page 78: ...he detector 4 Install compression fittings on each end of the tubing as described in Liquid line connections on page 2 21 5 Tighten the fittings at all connectors Connecting to a Radial Compression Mo...

Page 79: ...rmation about solvent selection and equilibration before use Delta Prep system The Delta Prep system column rack includes the necessary tubing clamps and clamp holders for mounting analytical and prep...

Page 80: ...ctions on page 2 21 5 Tighten the fittings at all column connectors Installing the prep column To install the prep column 1 Loosen the clamps at the prep column location and slide the column holders a...

Page 81: ...the left side of the Delta Prep system You can if you want place it on the column rack floor 2 Prepare the inlet tubing For an 8 10 mm small scale RCM prepare a length of 0 009 inch ID tubing to exte...

Page 82: ...Waters 2487 Detector requires the appropriate flow cell see the table titled Flow cell tubing sizes on page 2 22 and these preparations A 0 020 inch ID or 0 040 inch ID tubing to connect the LARGE SC...

Page 83: ...ip When using a Waters 2414 Detector with flow rates above 5 mL min use the flow splitter option The flow splitter eliminates excessive pressure on the RI cell It diverts about 1 of the flow to the RI...

Page 84: ...2 50 Installing the System...

Page 85: ...ntenance Caution To avoid instrument damage wait about 3 minutes after shutting down your system before you disconnect any interconnecting cables Contents Topic Page Troubleshooting 3 2 Performance te...

Page 86: ...rvice To expedite service provide the following information when you call Symptom Operating wavelength Detector sensitivity setting 0 001 to 2 00 AUFS Flow rate Type of column Operating pressure Sampl...

Page 87: ...ns General PrepLC troubleshooting Symptom Possible cause Corrective action Grinding or shuddering noise from pump high pressure shutdown not exceeded Blockage in system before transducer Clean pump he...

Page 88: ...not exceed 5 mL min 2414 2410 and 410 Detectors Do not exceed 100 psi for any Waters RI detector Replace detector flow cell if necessary see detector operator s guide Peak retention times halved Inco...

Page 89: ...hod to another You must therefore identify a pressure reference point Each time you start a new method record the system pressure Thereafter to diagnose a problem with system pressure compare current...

Page 90: ...correct the high pressure condition first isolate the part of the system in which the high pressure originates Gradual pressure increase Sample or mobile phase particulates can increase pressure grad...

Page 91: ...m Pressure reduced Pressure reduced Pressure reduced Pressure reduced Pressure reduced Adjust pressure transducer Replace pressure transducer Remove column replace w union run system Troubleshoot colu...

Page 92: ...the baseline is abnormal determine whether the variation is short or long term You can eliminate many causes of baseline abnormality by identifying the rate at which the baseline changes See the foll...

Page 93: ...e chromatography troubleshooting table Cycling Solvent not mixing properly Make sure correct pressure filter is installed Long term drift Wrong column equilibration Allow column to equilibrate Detecto...

Page 94: ...e pressure change Is the pressure higher or lower than the normal operating pressure Also it is important to observe whether the retention time changes act like this They appear suddenly at the end of...

Page 95: ...ile phase Problem Is operation Wrong column equilibration Equilibrate column No Yes Temp fluctuations Stabilize environment No Sparge conditions causing solvent components to evaporate at different ra...

Page 96: ...e Wrong degraded column Incorrect wavelength phase Solvent proportioning valve broken Troubleshoot pump See previous page Is pressure constant but different Is pump set to correct flow rate Change flo...

Page 97: ...peak pair In a gradient method if resolution of early peaks is poor but improves later in the chromatogram precolumn band broadening might be the problem If peak resolution is poor throughout the chro...

Page 98: ...mn by determining plate count low Replace column and check plate count low Inline filter or guard column clogged Clean replace filter or guard column Continued on next page Injector column tubing diam...

Page 99: ...as problem s cause Refer to the figure below to determine the possible cause of your column problem Continued from previous page Extra column band broadening Detector filter constant too high Adjust f...

Page 100: ...inlet frit Pressure reduced Determine plate count to verify performance Determine plate count Replace column outlet frit Retention time of marker compound changed Clean replace column and determine p...

Page 101: ...eal on page 3 58 Separation chemistry Check mobile phase and column Clogged solvent filter Replace filters Increased retention times Incorrect flow rate or solvent composition Change flow rate or solv...

Page 102: ...tor not allowed to warm up Allow detector to warm up until baseline is stable time varies based on wavelength and sensitivity Solvent contaminated Use fresh solvent Solvent not properly degassed rapid...

Page 103: ...Clean flow cell detector documentation Baseline noise short term 30 sec to 1 min cycling Inadequate solvent blending in pump Connect high flow mixer Flow fluctuating Stabilize flow Solvent not mixed...

Page 104: ...for excessive baseline noise Straight baseline no peaks No pump flow Set pump flow rate Lamp not on Troubleshoot detector Detector not zeroed Zero detector baseline Improper connection between Prep s...

Page 105: ...ow cell see detector documentation Analog output cable not properly connected between the Prep system and data system recorder or integrator Properly connect cable System grounded improperly Plug all...

Page 106: ...ction volume Sensitivity loss Leak in injector Troubleshoot injector Degraded contaminated or improperly prepared sample Use fresh sample Column contaminated Clean replace column Loss of column effici...

Page 107: ...cell windows Clean outside of flow cell windows General system troubleshooting Symptom Possible cause Corrective action Unit will not start Power cord not connected Check power cord No power at outlet...

Page 108: ...troubleshooting Symptom Possible cause Corrective action Pump will not run Loose control cable Reattach cable to rear of fluid handling unit High pressure limit set to 0 Set higher pressure limit on P...

Page 109: ...and disassemble fitting verify fitting components replace ferrule and other damaged parts Worn pump plunger seals Replace seals Loose pump head Tighten loose pump head s with a 5 32 inch hex head wren...

Page 110: ...to remove bubble Dirty check valve s Clean check valve s Faulty check valve s Replace check valve s Plugged solvent reservoir filter Clean or replace the filter Kinked or bent tubing Remove bend from...

Page 111: ...r troubleshooting Symptom Possible cause Corrective action Leakage Stator screws need tightening Tighten stator screws replace rotor seal Scratches on rotor seal Replace rotor seal Needle seal leakage...

Page 112: ...assed Sparge mobile phase Leaks at the fluid tubing connections Check for leakage at the connections with the corner of a tissue and tighten connection slightly if the tissue is moistened High pressur...

Page 113: ...not at 400 50 psi Set pump flow to achieve 400 50 psi Syringe contains a gas bubble usually seen at the top of the syringe Remove bubble Leaks at the fluid tubing connection Check for leakage at the...

Page 114: ...ge on DIRECT CONTROL screen External detector not calibrated Calibrate external detector External detector turned off after it has been identified on the bus RESCAN using the SYSTEM CONFIGURE screen D...

Page 115: ...Enter an improper value Use an unacceptable entry method RI detector troubleshooting Symptom Possible cause Corrective action Spikes on chart spikes are synchronous with pump pulses Solvent not proper...

Page 116: ...table currently in memory and the table number you entered display The table currently in memory will be replaced with the new table in the next step This message is accompanied by an audible alarm Re...

Page 117: ...udible alarm UV Detector 1 Not Found UV Detector 2 Not Found RI Detector Not Found Operation Device has disappeared from the IEEE 488 bus Check if the PowerLine module was turned on or if the PowerLin...

Page 118: ...stem resets the flow rate to 0 0 mL min Flow and composition appear on the display Invalid Injection Number The Injection Number is not part of the Step indicated Check the PROGRAM METHOD screen This...

Page 119: ...an obviously a system component remove the component from the system Then continue as follows Shutdown not caused by stop flow signal If a Stop Flow signal does not cause the shutdown or if you corre...

Page 120: ...ddress decoding bus latch and drive circuits Addresses at each RAM location associated address decoding bus latch and drive circuits Video RAM EEPROM location with interrupt read write associated addr...

Page 121: ...contact Waters Technical Service Extended tests After the automatic self diagnostic routine ends select the extended test routine by pressing the decimal key on the keyboard Perform the extended test...

Page 122: ...INJ input terminal on the rear panel External Switches and Hold Output tests Tests each of the four switch terminals and the Hold output terminal on the rear panel Chart test Produces a 0 to 10 mV sa...

Page 123: ...rerun the extended test routine or press any function key to resume normal operation Some of the extended tests require additional actions that require explaining These appear on the next several page...

Page 124: ...njector to start a run This test verifies that the INJ switch is functioning To perform an external inject test 1 Attach a jumper wire from INJ on the rear panel to a Gnd terminal on the rear panel se...

Page 125: ...d to INJ If you want to bypass the Hold Output test press ENTER Hold output test To prevent further injections in case of power failure the Hold switch outputs a signal to devices that can recognize t...

Page 126: ...shows you how to adjust transducer slightly Do this if you experience high or low pressure shutdowns to determine that the pressure transducer is causing your problem Tip Turn the screw slowly because...

Page 127: ...lets you evaluate the system when you suspect a defective proportioning valve is causing erratic chromatographic results You can perform the test in less than 1 hour Use pure methanol as the mobile ph...

Page 128: ...order to 0 3 Pump solvent 2 reservoir C or D isocratically at 5 mL min and adjust the recorder to full scale using the recorder s variable full scale input The recorder is now set to respond so that 0...

Page 129: ...1 change in composition Evaluate results The figure Test results with all valves working on page 3 46 is typical of the results obtained from this test when all valves are working Valve failure A valv...

Page 130: ...3 46 Troubleshooting Testing and Maintenance Test results with all valves working...

Page 131: ...3725i injectors Fuses Column rack tubing configuration The column rack does not typically require maintenance However the figure below illustrates the tubing configuration inside the column rack in ca...

Page 132: ...perating the unit Fluid handling unit maintenance This section describes the maintenance or repair procedures for the fluid handling unit These procedures include Pressure transducer calibration Check...

Page 133: ...ld be a positive value slightly greater than 0 psi Tip The pressure value can read 0 psi even when the pressure transducer is not set properly because the screen does not display negative pressure Tip...

Page 134: ...display reads 0 to 100 d Move the screwdriver to the center hole Turn the screwdriver slowly until a small positive value appears e Replace the cover screw in the left hole Cleaning and replacing che...

Page 135: ...rate to 3 0 to 4 0 mL min and purge for 10 minutes 3 Replace the contents of the solvent reservoir with water 4 Set the flow rate to 3 0 mL min and purge for 10 minutes Replacing check valves If the...

Page 136: ...nlet check valve assembly Caution To protect the parts from contamination use forceps or tweezers to handle the parts after cleaning them and when reassembling the inlet check valve PUMP HEAD HOUSING...

Page 137: ...pump head 8 Screw the assembly up into the pump head being careful to not tip the housing 9 Firmly tighten the inlet check valve and attach the tubing To disassemble outlet check valves 1 Shut down t...

Page 138: ...ump head 3 Place the seat assembly into the pump head Face the shiny side upward Caution To protect the parts from contamination use forceps or tweezers to handle the parts after cleaning them and whe...

Page 139: ...ads require a dual outlet check valve shown in exploded view in the figure Dual check valve assembly on page 3 56 1 If the flushing procedure in Cleaning check valves on page 3 51 does not sufficientl...

Page 140: ...oller and disconnect the power cord The proportioning valve stops all solvent lines 2 Disconnect the inlet line from the inlet check valve If necessary use a 5 16 inch wrench to loosen the inlet line...

Page 141: ...lacing the pump seal on page 3 58 Tip If you are replacing the pump plunger or the wash seal refer to the next procedure to remove the head support assembly Removing the head support assembly The figu...

Page 142: ...ger wash seal on page 3 65 Replacing the pump seal During routine maintenance replace the seal in both pump heads at the same time Tip The seal insertion tool that this procedure refers to consists of...

Page 143: ...tip of the insertion tool so that the open end of the seal with the spring faces out from the end of the tool b Fit the guide into the recess at the rear of the pump head Tip The circular opening in...

Page 144: ...Place the three plunger bearings behind the seal in the pump head as follows Bearing 1 s grooved side faces the rear of the pump head Bearing 2 s grooved side faces the front of the pump head Bearing...

Page 145: ...dexterity as well as a special plunger insertion tool Contact your Waters Service Representative before performing it The plunger may experience excessive wear if you do not use the plunger wash If y...

Page 146: ...he cap and pull it toward you Exposed plunger and piston 4 Insert the plunger insertion tool into the piston cavity With one hand force the inner part of the plunger insertion tool against the snap ri...

Page 147: ...enance procedures 3 63 Using the plunger insertion tool and snap ring pliers to remove the plunger 5 Pull the plunger straight out of the cavity Removing the plunger Snap ring pliers Plunger insertion...

Page 148: ...the end of the piston Tip Seat the entire snap ring in the groove in the piston Otherwise it can spring out of position when you release the pliers 9 Remove the pliers and plunger insertion tool The...

Page 149: ...he head support assembly To replace the plunger wash seal 1 Remove the pump head and head support assembly 2 Remove the indicator rod from the head support assembly 3 Push on the wash seal from the ba...

Page 150: ...Replace the retainer on the front of the head support assembly 5 Insert the indicator rod into its hole in the back of the head support assembly Make sure the spring and PTFE washer are on the rod 6...

Page 151: ...slightly to correct the alignment 13 Reconnect the solvent lines and examine them for leaks Replacing fuses This section includes procedures for replacing fuses on the rear panel of the controller and...

Page 152: ...se holder out as though opening a drawer Spare fuses are in the Startup Kit and or in the fluid handling unit shipping box 4 Install the correct fuses in the holder The arrow on each fuse holder point...

Page 153: ...the controller Replace this fuse with a 1 5 A fuse Startup Kit Auxiliary 12 VAC and pump power fuses To replace the auxiliary 12 VAC fuse 1 Insert a small flat blade screwdriver into the fuse holder...

Page 154: ...e operating voltages are 120 220 VAC 4 A and 125 VAC IEC time delay 5 20 mm 6 Insert the new fuse and holder back into the fuse chamber on the rear panel 7 Lock the fuse holder into place using the sc...

Page 155: ...back into its location on the rear panel of the fluid handling unit 6 Lock the fuse holder in place using the screwdriver Maintaining rheodyne manual injectors Rheodyne manual injectors require minim...

Page 156: ...he water in the syringe into the injector Notice the lack of resistance to syringe discharge 2 Repeat step 1 with the injector handle halfway between Load and Inject the pump must be off The resistanc...

Page 157: ...or seal on page 3 74 Rheodyne 7725i injector exploded view Handle screw Handle Needle guide Set screws 2 Pressure adjusting screws Body Thrust bearing Spring washers 4 Rotor pin Position sensing switc...

Page 158: ...l markings on the body and the painted spot on the adjusting screw to gauge how far to tighten the screw 5 If the new setting fails to accomplish leak free operation repeat the procedure by an additio...

Page 159: ...ou need to remove the injector from the front panel remove the knob 2 Remove the three stator screws 3 Remove these parts by pulling axially a Stator and stator face assembly remove together If the st...

Page 160: ...ly fit into the mating holes in the stator only one way 5 Install the stator and stator face assembly on the valve so that the pin in the stator ring enters the mating hole in the stator 6 Alternately...

Page 161: ...des also include the hazard symbols with accompanying text statements describing the hazards and telling you how to avoid them This appendix presents all the safety symbols and statements that apply t...

Page 162: ...electric shocks ultraviolet radiation exposures and others When the following symbols appear in a manual s narratives or procedures their accompanying text identifies the specific risk and explains ho...

Page 163: ...ing Risk of explosion Warning Risk of eye injury Warning Pressurized nonmetallic or polymer tubing can burst Observe these precautions when working around such tubing Wear eye protection Extinguish al...

Page 164: ...Ensure that the nitrogen supply pressure never falls below 690 kPa 6 9 bar 100 psi during an analysis in which flammable solvents are used Also ensure a gas fail connection is connected to the LC syst...

Page 165: ...nisms and other biological materials To avoid infection with these agents assume that all biological fluids are infectious observe Good Laboratory Practices and consult your organization s biohazard s...

Page 166: ...ler le droit de l utilisateur exploiter l quipement Achtung Jedwede nderungen oder Modifikationen an dem Ger t ohne die ausdr ckliche Genehmigung der f r die ordnungsgem e Funktionst chtigkeit verantw...

Page 167: ...e trouvant proximit de l instrument Evitez d utiliser des tubes s v rement d form s ou endommag s Evitez d utiliser des tubes non m talliques avec du t trahydrofurane THF ou de l acide sulfurique ou n...

Page 168: ...iamenti nei tubi non metallici riducendo notevolmente la pressione di rottura dei tubi stessi Advertencia se recomienda precauci n cuando se trabaje con tubos de pol mero sometidos a presi n El usuari...

Page 169: ...Warnings that apply to all Waters instruments A 9 Nonmetallic Tetrahydrofuran THF Methylene chloride Dimethyl sulfoxide THF...

Page 170: ...tueuses Vorsicht Der Benutzer wird darauf aufmerksam gemacht dass bei unsachgem er Verwenddung des Ger tes die eingebauten Sicherheitseinrichtungen unter Umst nden nicht ordnungsgem funktionieren Atte...

Page 171: ...l instrument Vorsicht Zum Schutz gegen Feuer die Sicherungen nur mit Sicherungen ersetzen deren Typ und Nennwert auf den Tafeln neben den Sicherungsabdeckungen des Ger ts gedruckt sind Attenzione per...

Page 172: ...e can appear in instrument user manuals and on the instrument s front or rear panels Electrical power on Electrical power off Standby Direct current Alternating current Protective conductor terminal F...

Page 173: ...ng symbols A 13 Handling symbols These handling symbols and their associated text can appear on labels affixed to the outer packaging of Waters instrument and component shipments Keep upright Keep dry...

Page 174: ...A 14 Safety Advisories...

Page 175: ...range 0 to 100 programmable in 1 increments for each of four reservoirs A B C and D Total composition must sum to 100 Compositional accuracy Better than 3 0 Automatic solvent Sparging Standard helium...

Page 176: ...lay screens Cursor movement keys simplify programming editing and parameter entering All keys are solvent resistant Programmable timed events Fifteen timed events can be programmed and stored for each...

Page 177: ...A maximum current Hold output One open connector switch closure to ground Maximum current sink 40 mA Low output indicates pumps stopped due to Exceeding high pressure limit Below low pressure limit A...

Page 178: ...urface material 316 stainless steel ruby sapphire fluorocarbon polymer System controller Height 7 19 inches 18 26 cm Depth 21 75 inches 55 25 cm Width 11 32 inches 28 75 cm Weight 42 pounds 19 1 kg Fl...

Page 179: ...Item Recommended stock Part number Valve 3 way purge 0 700001309 System interface cable 0 WAT088972 3725 injector Item Recommended stock Part number 3725 Rebuild Kit 1 201000116 Stainless Steel Needle...

Page 180: ...WAT033326 Plunger Assembly 2 700002123 Plunger Seal Kit 2 WAT037490 Gradient Proportioning Valve Assembly 0 WAT082823 300 mL configuration Item Recommended stock Part number 300 mL Conversion Kit 0 2...

Page 181: ...Contents Topic Page Clean solvent D 2 Solvent miscibility D 3 How to use miscibility numbers M numbers D 5 Buffered solvents D 6 Solvent head height D 6 Solvent viscosity D 6 Solvent degassing D 7 So...

Page 182: ...e information Inlet solvent filters can be used at low flow rates To avoid drawing foreign particles into the pump where they can accumulate and affect pump operation keep the solvent reservoir filter...

Page 183: ...nic solvents When switching from a strong buffer to an organic solvent flush the buffer out of the system with distilled water before adding the organic solvent Also when using a strong buffer flush a...

Page 184: ...5 Cyclohexanone 2 24 155 7 28 210 4 5 Nitrobenzene 2 03 210 8 14 20 4 6 Benzonitrile C 22 19C 1 15 19 4 8 Dioxane C 54 10C 3 17 220 5 2 Ethanol C 20 78 3 14 210 5 3 Pyridine 0 94 115 3 16 305 5 3 Nit...

Page 185: ...d degree of miscibility For example ethers or tertiary amines show unpredicted miscibility with hydroxylic solvents due to hydrogen bonding Unusually strong hydrogen bonding is also responsible for th...

Page 186: ...illi Q water containing 0 2 sodium azide Use a syringe to flush distilled water through the vent holes while running the pump After flushing with water flush the pump with 10 methanol before shutdown...

Page 187: ...t where the intermolecular attractive forces between molecules of the solvent are similar to those of the gas like dissolves like If the main attractive forces are Van der Waals forces the gas is more...

Page 188: ...ted a 95 reduction in sensitivity of the fluorescence of borate benzoin complex in air equilibrated ethanol The oxygen quenching varies with different types of compounds and aromatic hydrocarbons alip...

Page 189: ...re partial pressure of helium Vacuum alone is too slow as an acceptable means of degassing solvent In the techniques listed above except for helium sparging the solvent reequilibrates to air saturatio...

Page 190: ...D 10 Solvent Considerations...

Page 191: ...e Table Currently Executing message 3 32 caution symbol A 5 Chart and Press switches 1 10 Chart test 3 41 Chassis ground terminal 1 11 Check Corresponding Table message 3 33 Check valves cleaning 3 50...

Page 192: ...lit 3 30 troubleshooting 3 30 RI 3 31 UV 3 30 Digital input signal 1 10 Display screen 1 16 Doubled retention times 3 17 E EC Authorized Representative vi Electrical connections AC power 2 15 IEEE 48...

Page 193: ...26 system 3 23 3 24 Head support removing 3 57 Help 3 2 online 1 19 High system pressure 3 5 considerations 3 6 Hold Output test 3 41 Hold signal 1 10 HOME key 1 16 I IEEE 488 address test 3 42 IEEE 4...

Page 194: ...65 3 67 pump head removal 3 56 pump plunger replacement 3 61 3 67 pump seal replacement 3 58 replacing 5 A fuse 3 70 3 71 replacing auxiliary power fuse 3 69 replacing operating voltage fuse 3 67 mass...

Page 195: ...et port Delta Prep system 1 5 Purge valve 1 5 1 12 Delta Prep system 1 5 purpose and audience iv R Rack column 1 12 Radial Pak cartridges 1 14 Random baseline noise 3 21 Rapid baseline drift 3 18 Rear...

Page 196: ...3 19 Small scale flow path 1 12 Small scale sample injection valve option 2 40 Software troubleshooting 3 31 shutdown messages 3 34 warning messages 3 32 3 34 Solvent considerations clean D 2 degassin...

Page 197: ...0 V Values entering 1 17 Viscosity D 6 W Warning messages 3 32 3 34 Can t Save Table Currently Executing 3 32 Check Corresponding Table 3 33 First Vial Greater Than Last Vial 3 34 Illegal Vial Number...

Page 198: ...Index 8 Waters Technical Service contacting 3 2 Workstations Empower 2 15 MassLynx 2 15...

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Waters HPLC, Installation And Maintenance Manual

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Summary of Contents for HPLC

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