1. Manuals
  2. Brands
  3. Waters Manuals
  4. Laboratory Equipment
  5. Prep Series
  6. Installation and maintenance manual

Waters Prep Series Installation And Maintenance Manual

Hide thumbs
Table of Contents

Advertisement

Quick Links

Waters Prep Series
Installation and Maintenance Guide
71500045204/Revision B
Copyright © Waters Corporation 2010
All rights reserved

Advertisement

Table of Contents
loading
Need help?

Need help?

Do you have a question about the Prep Series and is the answer not in the manual?

Questions and answers

Related Manuals for Waters Prep Series

Summary of Contents for Waters Prep Series

  • Page 1 Waters Prep Series Installation and Maintenance Guide 71500045204/Revision B Copyright © Waters Corporation 2010 All rights reserved...

  • Page 2: Copyright Notice

    Corporation assumes no responsibility for any 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 damages in connection with, or arising from, its use.

  • Page 3: Customer Comments

    Contacting Waters ® Contact Waters with enhancement requests or technical questions regarding the use, transportation, removal, or disposal of any Waters product. You can reach us via the Internet, telephone, or conventional mail. Waters contact information Contacting medium Information...

  • Page 4: Safety Advisories

    Australia C-Tick EMC Compliant Confirms that a manufactured product complies with all applicable United States and Canadian safety requirements Consult instructions for use Audience and purpose ® This guide is intended for personnel who install and maintain the Waters Prep Series HPLC system.

  • Page 5: Intended Use Of The Waters Prep Series Hplc System

    Intended use of the Waters Prep Series HPLC system Use the Waters Prep Series HPLC system to isolate and purify a wide variety of samples. The Waters Prep Series HPLC system is for research use only. Calibrating To calibrate LC systems, follow acceptable calibration methods using at least five standards to generate a standard curve.

  • Page 6: Ec Authorized Representative

    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: Table Of Contents

    Safety advisories ....................iv Operating this instrument ................. iv Applicable symbols ..................... iv Audience and purpose..................iv Intended use of the Waters Prep Series HPLC system ........v Calibrating ......................v Quality-control ..................... v ISM classification ....................v ISM Classification: ISM Group 1 Class B ............v EC authorized representative ................
  • Page 8 Installing the small-scale sample injection valve option (PrepLC system) 2-40 Using an autoinjector ..................2-41 Making electrical connections ............... 2-41 Connecting liquid lines when using a Waters autoinjector ......2-41 Connecting a fraction collector ..............2-42 Making the remote start connection............. 2-42 Making chart mark connections ..............
  • Page 9 Warning symbols ....................A-2 Task-specific hazard warnings................ A-2 Specific warnings ..................... A-3 Caution symbol ....................A-5 Warnings that apply to all Waters instruments ......... A-6 Electrical and handling symbols ..............A-12 Electrical symbols ..................A-12 Handling symbols ..................A-13 Table of Contents...
  • Page 10 B Specifications ..................B-1 C Spare Parts .................... 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 degassing ....................

  • Page 11: Overview

    Overview Waters produces its Prep Series high performance liquid chromatography (HPLC) systems in two configurations: • Waters PrepLC™ System • Waters Delta-Prep™ System Although the two systems share many features, certain aspects Tip: nevertheless differ. This guide addresses both differences and...

  • Page 12: Waters Prep Series

    Waters Prep series The Waters Prep Series offers these features: • Two pump configurations: flow rate with 500-µL pump heads at 4000 psi – 150-mL flow rate with 1000-µL pump heads at 2000 psi – 300-mL μ Fitted with 1000-...

  • Page 13: Delta-Prep System

    Controller Fluid handling unit Delta-Prep system The Waters Delta-Prep system is an HPLC system capable of analytical and preparative scale chromatography. Use the system’s pump with either 500- or 1000-µL volume heads. The 500-µL pump heads permit flow rates of 1 to 150 mL/min, and the 1000-µL heads permit flow rates of 4 to 300 mL/min.

  • Page 14: Delta-Prep

    Waters Delta-Prep system Controller 2487 detector Column rack Fluid handling unit Drip tray Drip tray Delta-Prep system components PrepLC System controller – Houses system electronics and controls the solvent gradient, flow rate, sparging, and external events. It also provides connection terminals and communication ports for operating with external devices.

  • Page 15: Waters Prep Series Modules

    Rheodyne 3725i injector – For large-scale injections, incorporates a 20-mL fixed sample loop, though you can install loops of varying injection volumes. Optional loops, available from Waters, handle fixed volumes from 2 to 20 mL. Purge valve – Lets you divert pump output to waste (e.g., when purging the system) or through the injector, columns, etc.
  • Page 16 Waters Prep series fluid handling unit Solvent reservoir lines (4) Outlet check Plunger wash valves (2) inlet line Inlet check valves (2) Connectors and fittings Manual sample drawer inlet valve Drip tray Pump head Fluid metering Solvent selection and proportioning take place on the low pressure (intake) side of the solvent delivery system.
  • Page 17 The wash pump runs whenever 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 solvent composition, flow rate, sparging, and external events, during a run. PrepLC controller front panel...
  • Page 18 PrepLC controller rear panel AC power inlet Pump fuse Auxiliary fuse Plug-in terminal receptacles Pump interface connector IEEE-488 RS-232 connector connector Rear panel This section describes the electrical connections to the controller’s rear panel. Do not use cables longer than 9.8 feet (3 meters) when you Caution: connect to the screw-type barrier terminal strips.

  • Page 19: Inject Start

    Hold (Connect Hold and Gnd) – Produces an output signal that prevents further injections in cases of catastrophic events: power failure, pressure shutdown, or when abort conditions arise. Connect it with any compatible device that must be stopped when any of these events happen. Waters Prep series...

  • Page 20: Waters 746 Integrator

    Tip: in a Waters workstation” on page 2-16) or connect them in series. Thus you might connect the 7725i injector, a Waters non-PowerLine autoinjector, and a Waters 746 integrator. An autoinjector connected to this terminal starts the run. (Waters Tip: autoinjectors start the run through PowerLine control.) The time required to...

  • Page 21: Chassis Ground

    IEEE-488 – Allows communication interface between system controller and PowerLine detectors and autoinjectors. RS-232 – Allows communication interface for Waters 746 integrator or Waters MassLynx™ or Empower™ workstations. Injectors Use the Rheodyne 3725i injector for large-scale separations and the 7725i model for small-scale ones.
  • Page 22 For large-scale operations, inject sample through the manual pump inlet line, the Rheodyne 3725i injector, or any available solvent delivery line. Rheodyne 3725i injector The Rheodyne 3725i injector incorporates a 20-mL fixed sample loop. The loop volume and its valve passages precisely determined sample volume. Column rack (Delta-Prep system) The column rack (see the figure “System column rack (Delta-Prep system)”...

  • Page 23: Accessories

    Several Waters Prep Series options let you to expand your system’s capability. Waters fraction collector You can program controller event options to integrate a Waters Fraction Collector as part of the Waters Prep Series. You can program the fraction collector itself for maximum flexibility and productivity. SE 120 chart recorder The SE™...

  • Page 24: Getting Started

    Flow splitter option The flow splitter option modifies the Prep Series for high flow rate use with a refractive index detector. It splits eluent flow so that 1% goes to the refractometer and 99% to the UV detector or fraction collector. This serves the necessary purpose of minimizing solvent pressure on the RI cell.
  • Page 25 Diagnostic tests The PrepLC controller is shipped as a PowerLine controller. Accordingly, the Startup screen appears in PowerLine mode. The self-diagnostics test each PowerLine module in the Waters Prep Series. These modules include: • Controller and pump •...

  • Page 26: Using The Front Panel

    Detector or autoinjector failure If a detector or the autoinjector fails the diagnostics test, the Startup screen indicates so. Turn the controller off, then on again. If it fails again, call Waters Technical Service. Leaving the Startup screen To leave the Startup screen, press any function key. Function keys are explained in “Function keys”...
  • Page 27 • ENTER – Registers the value you type for a parameter. The system evaluates each entry to determine whether it is within the proper limits. An error message appears when the value is not allowed. • CLEAR – Erases the value typed immediately beforehand, if you did not press ENTER.
  • Page 28 Screen keys The five unlabeled screen keys are directly below the display screen. Labels appearing at the bottom of displayed screens, directly above each screen key, indicate the keys’ functions, which vary from screen to screen. Some screens, like the OPERATE METHOD and OPERATE GRADIENT screens, display the MORE screen key.

  • Page 29: Displaying Help

    Press the RETURN screen key to quit Help. Shutting down the system If you do not plan to use the Waters Prep Series system for overnight or longer, shut the system down, observing these precautions: • Do not leave buffers in an unused system. First, flush the lines with Milli-Q HPLC-grade water.
  • Page 30 Uses a Method table that links time-based control tables. These include a Gradient table, Event table, and Detector table. The controller communicates with the PowerLine modules (autoinjector and detectors) through the IEEE-488 interface. It communicates with the Waters 746 integrator through the RS-232 serial interface. Operation...
  • Page 31 – Methods specifying vial numbers – Number of injections from each vial – Injection volume The controller can contain 15 sets of Method tables. Each set of tables can contain these individual tables: • Gradient – Includes up to 15 operational steps that define the varying solvent composition, flow rate, time range, and rate of change for each phase of the gradient.
  • Page 32 In gradient configuration, the controller does 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 sets of tables.
  • Page 33 Pump Program Program Initiate Isocratic setup gradient op grad event screen screen screen screen screen Pump Operate config gradient screen screen See the Waters Prep Series Operator’s Guide for details about configuring and operating the Gradient controller. Getting started 1-23...
  • Page 34 1-24 Overview...

  • Page 35: Installing The System

    Installing the System Contents Topic Page Setting up and inspecting Electrical requirements Assembling the system 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 collector 2-42 Installing analytical and preparative columns 2-43...

  • Page 36: Setting Up And Inspecting

    Remove the system components from their respective cartons, and place them at the installation site. Inspect all items for shipping damage. Immediately report any damage to both the shipping company and your Waters Technical Service representative. Installing the System...

  • Page 37: Selecting The Site

    Selecting the site This section describes the physical and environmental requirements of your Prep system. PrepLC system Install the system away from direct sunlight and heating and cooling vents. These additional conditions must apply: • Temperature ranges from 4 to 38 °C (39 to 100 °F). •...
  • Page 38 Place the assembly in position on the bench. Place the fluid handling unit in the bottom section of the shelf unit (see figure “Waters Delta-Prep system dimensions” on page 2-4). Before installing the controller, determine whether you must...

  • Page 39: Electrical Requirements

    Electrical requirements This section describes the Prep system’s electrical configurations. To avoid electric shock, make sure the power cord is Warning: disconnected from the rear panel of the instrument before performing this section’s procedures. Electrical conditions The system requires these electrical conditions: •...
  • Page 40 Changing the voltage setting 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 to step 8.

  • Page 41: Assembling The System

    Assembling the system This section explains how to connect the Rheodyne injectors and the optional M-1000 PrepPak module to the controller and the controller to the fluid handling unit. It also describes additional, rear panel connections. Externally generated voltages can damage the instrument. Caution: Shorting the 12-VAC terminal to ground or and event output causes the +12 VAC fuse to blow.
  • Page 42 Injector electrical connector Injector electrical connector Delta-Prep system To electrically connect the Rheodyne 7725i and 3725i 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 CHART + PRESSURE +...

  • Page 43: Connecting The M-1000 Preppak Module (Optional)

    Connecting the M-1000 PrepPak module (optional) The M-1000 PrepPak module generates an output that causes the controller to abort pump action when radial compression in its chamber falls below 650 psi. To connect the optional M-1000 PrepPack: Connect the signal output to the Stop Flow terminal on the controller’s rear panel.
  • Page 44 integrator or chart recorder plots the signal. The full-scale range of the chart outputs is +10 mV full scale. Tips: • The integrator must invoke expanded memory to use the second channel on the 746 integrator to plot pressure or percent composition. It plots the second channel after the first channel finishes.
  • Page 45 Pressure output The Pressure output monitors pump pressure during ramp testing and other service procedures. It also monitors how different solvents affect pressure during various phases of gradient operation. The full scale range of the pressure output is +10 mV. Plotting Connect the leads at one end of the event cable (Startup Kit) to the Pressure+ and Pressure–...
  • Page 46 External device connections CHART + PRESSURE + +5 VAC switch closure or TTL device PRESSURE — CHART — +12 VAC auxiliary power To connect external devices requiring +12 VAC auxiliary power: Connect one end of a two-conductor cable between the device and the controller to the appropriate +/–...

  • Page 47: Attaching The Interface Cable And Power Cord

    To connect fraction collectors, see “Connecting 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 devices, consult the documentation supplied with the detector.
  • Page 48 Attaching the pump interface cable To avoid damaging the PrepLC controller and/or pump, make Caution: sure the controller power switch is turned off before performing this procedure. To attach the pump interface cable: Shut down the controller. Connect the 37-pin interface cable to the pump interface connector on the controller rear panel (see the figure “Pump interface cable and power cord locations”...

  • Page 49: Connecting Ieee-488 Interfaces

    Performing 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 information from the data system. Set up the controller for gradient operation. The data system operates as the system controller on the IEEE-488 interface.
  • Page 50 Stacked IEEE-488 connections in a Waters workstation busLAC/E card (Empower) or GPIB card (MassLynx) PrepLC Data system controller (as gradient controller) IEEE-488 cable IEEE-488 connector PrepLC 717plus 2487 controller Autosampler Detector (as gradient controller) IEEE-488 connections in a Waters data network IEEE-488 IEEE-802.3...
  • Page 51 IEEE-488 interface to communicate with the PowerLine devices (where the PowerLine controller is the controller on the IEEE-488 interface). Set up the PrepLC as a PowerLine controller. To ready the PrepLC controller as a PowerLine controller, see the Waters Prep Series Operator’s Guide. Supported PowerLine devices include the following: •...
  • Page 52 Connect the other end of the cable, using the stackable connector for interconnecting additional instruments, to the IEEE-488 connector on the next PowerLine instrument. If using a multicomponent configuration, connect a second IEEE-488 cable to the stackable connector on the PowerLine instrument. Connect the other end of the cable to the IEEE-488 port on the next PowerLine component.
  • Page 53 Data system startup sequence This sequence requires you to start all devices in your data system Tip: operating before you start the computer. As you start each component, wait briefly to allow its internal diagnostic tests to run. This ensures each module functions and quickly identifies failures.

  • Page 54: Connecting To The Waters 746 Data Module

    Shut down the other IEEE-488 devices. Connecting to the Waters 746 data module You can use the RS-232 interface to connect the controller to a Waters 746 Data Module. The interface transmits this data using: • Control commands from the data module to the controller •...

  • Page 55: Liquid Line Connections

    Liquid line connections The Waters Prep system Startup Kit includes a variety of tubing and fittings for connecting to the fluid handling unit, injector, detector, and column. Refer to the list in the Startup Kit for information on all included tubing and fittings.
  • Page 56 For flow rates greater than ~10 mL/min and for large-scale operation, connect the column outlet to the sample side of the detector cell with 0.040-inch ID tubing. The table below shows tubing sizes for the various flow cells used in Waters UV detectors. Flow cell tubing sizes...
  • Page 57 PrepLC system fluid pathway Large-scale injector Purge Plunger seal outlet wash solvent PrepLC pump Plunger seal wash pump figure “Delta-Prep system fluid pathway” on page 2-24 shows the fluid pathway in the Delta-Prep system. Assembling the system 2-23...
  • Page 58 Delta-Prep system fluid pathway Plunger seal Small-scale injector wash solvent Scale select Solvents valve Large-scale injector PrepLC pump Purge outlet Fraction Plunger seal valve wash pump Recycle to pump Fractions/waste/recycle valve Cutting stainless steel tubing When cutting tubing, avoid angled cuts. These create a bad fit between the tubing and connector port, which creates eddies (unswept volume) at the junction.
  • Page 59 Installing fittings To install fittings: Slide the fitting and then the ferrule (large end of the taper first) over the end of the tubing. Compression screw assembly Ferrule Tubing (Cut must be perpendicular to the tubing axis.) Bottom the tubing and ferrule in the fitting seat. As you press the tubing into the connector, tighten the compression screw 3/4 of a turn beyond finger tightness.
  • Page 60 System sparge and helium setup • Seal wash setup • Rheodyne injector connections figure “Waters Prep series fluid handling unit” on page 1-6 shows the fluid handling unit. Solvent reservoir caps Limit the solvent system to 5 psi pressure when you use Caution: pressurized solvent containers.
  • Page 61 Solvent reservoir caps The caps provided with the system fit 4-liter reservoirs, which Waters recommends. You can, however, obtain caps that fit 1-liter reservoirs. Choose solvent reservoirs onto which caps fit snugly.
  • Page 62 The filters press onto the ends of the solvent inlet lines. Their large-pore size and surface area help the pump operate effectively at preparative flow rates. To connect a solvent reservoir to the fluid handling unit: Push a labeled solvent tube through a hole in the cap of a correspondingly labeled reservoir.
  • Page 63 Attach an eluent filter or L-shaped tube (both in Startup Kit) to the solvent line. The tubing must stop against a ridge inside the eluent filter. Forcing tubing into the filter by pushing it beyond this ridge Caution: can create these problems: •...

  • Page 64: Connecting A Helium Tank To The Fluid Handling Unit

    Connect the other end of the vent tube to an eluent filter (see the figure “Solvent reservoir filter and diffuser placement” on page 2-28). Place the filter end of the vent tube in a fume hood. Insert the solvent reservoir cap into the top of the reservoir. Repeat steps 1 to 4 for each solvent reservoir.

  • Page 65: Sparging

    Sparging Sparging minimizes dissolved gases in the solvent. This decreases the potential for degassing when different mobile phases mix in the gradient proportioning valve. The helium flow through the system is as follows: • The helium is introduced into the solvent through a diffuser, which disperses the gas into small bubbles.
  • Page 66 Shutoff valve assembly 0.020 or 0.040-inch ID 1/4 NPT M × 1/8 NPTF 1/8 NPT × Z fitting SS tubing bushing (optional) To regulator or To sparge Fitting house helium supply Shutoff valve Ferrule 1/8 NPT × 1/8 NPT Ferrule Compression nipple screw...

  • Page 67: Setting Up The Plunger Wash

    Sparge gas inlet connection CAUTION DO NOT REMOVE CABLE WHILE UNIT IS POWERED CONNECT TO 4000 CONTROLLER ONLY 0.5A Sparge FUSE inlet connection Setting up the plunger wash Caution: • You must set up the plunger wash when you initially install the fluid handling unit.

  • Page 68: Considerations

    Considerations Use a solvent that is miscible with your mobile phase and which contains no dissolved salts that could crystallize as it evaporates. Also, empty and refill the plunger wash reservoir with new solvent about once a month (more often when used frequently) if you reuse it.

  • Page 69: Connecting To The Injection Panel (Preplc System)

    Put the inlet tube back into the wash solvent reservoir. Connecting to the injection panel (PrepLC system) Refer to the figure “Injector panel (PrepLC system)” on page 1-13 when Tip: following the procedure in this section. Connecting to the purge valve and Rheodyne 3725i injector The pump outlet connects to the injection panel with 0.020-inch ID tubing.
  • Page 70 0.009-inch ID tubing between the injector and the small-scale column. Use 0.020-inch ID tubing throughout the system for flow rates above 10 mL/min to maintain adequate backpressure. Tip: Waters offers optional small-scale injector and scale select valves for the PrepLC system. Contact your local Waters Technical Service representative for details.

  • Page 71: Connecting To The Column Rack (Delta-Prep System)

    Pump outlet connection to the prep column (Large-scale use) Injector panel Column outlet To detector Column inlet Pump outlet line Connecting to the column rack (Delta-Prep 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 other.
  • Page 72 System column rack (Delta-Prep system) Small-scale injector Small/large-scale switching valve Vials Large-scale Inlet (from pump) injector Purge outlet Purge/ system valve Cabinet latch Inlet (from detector) Fraction outlets 1-8 Fraction outlets selector Small-scale column outlet Large-scale column outlet Waste Recycle to pump TP01471 Fractions/waste/recycle valve Before you connect to the column rack, consult the table below for material...
  • Page 73 Column rack connections (Continued) Column rack Type of Tubing ID Connect to connection tubing Purge outlet Stainless 0.040 Waste container Fraction PTFE 0.062 Fraction containers outlets Waste PTFE 0.062 Waste container The fluid handling unit connects to the column with a 0.040-inch ID tubing (Startup Kit) installed between the pump outlet and the Inlet bulkhead connector on the column rack’s front panel.

  • Page 74: Installing Sample Injection Options

    Installing the small-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. This kit includes these components: • Rheodyne 7725i variable-volume injector valve assembly •...

  • Page 75: Using An Autoinjector

    Tip: to the column rack in the Delta-Prep system convenient. Connecting liquid lines when using a Waters autoinjector To bypass the Rheodyne injector connecting inlet and outlet lines: Locate the autoinjector to the system’s left side, allowing space to access the solvent reservoirs.

  • Page 76: Connecting A Fraction Collector

    Connect pins 9 and 10 on the collector to the appropriate input terminals on the detector. Here are two examples: • Connect to the Mark +/– terminals on the Waters 2487 or 2414 Detector. • Connect to any available Event In and Gnd terminals on the Waters 490 Detector.

  • Page 77: Installing Analytical And Preparative Columns

    Program the Mark function in the detector. Installing analytical and preparative columns This section describes how to install analytical and preparative columns in both the PrepLC and Delta-Prep systems. PrepLC system The PrepLC system includes clamps and clamp holders for mounting a column vertically onto the shelf unit.
  • Page 78 Install compression fittings on each end of the tubing as described in “Liquid line connections” on page 2-21. Tighten fittings at all connectors. Using an M-1000 PrepPak module To use M-1000 PrepPak module: Assemble the M-1000 PrepPak module as described in its operator’s guide.

  • Page 79: Delta-Prep System

    Tighten the fittings at all column connectors. Column and cartridge preparation See the Care and Use Manual that accompanies your column or cartridge for specific information 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 preparative columns.
  • Page 80 Installing an analytical column To install an analytical column: Loosen the clamps at any available column location and slide the column holder apart. Slide the column in place and tighten the clamps to secure it in position. Prepare a length of 0.009-inch ID tubing to extend between the connector labeled Small Scale –...
  • Page 81 Place the PrepPak module inside the column rack, between the prep and analytical column holders. Prepare a length of 0.040-inch ID tubing to extend between the connector labeled Large Scale – To Column Inlet and the column inlet (bottom end cap). Prepare another to extend between the connector labeled Large Scale –...

  • Page 82: Making Detector Connections

    This section describes connecting the column outlet to the detector in the PrepLC and Delta-Prep systems for large-scale and small-scale operation. PrepLC or Delta-Prep system Small-scale operation with a Waters 2487 Detector and semi-prep or prep flow cell requires these preparations: •...

  • Page 83: Using The Ri Detector With The Flow Splitter Option

    Your detector type determines whether you do this by interchanging two BNC signal cables or by keyboard input. Using the RI detector with the flow splitter option When using a Waters 2414 Detector with flow rates above 5 mL/min, use Tip: the flow splitter option.
  • Page 84 2-50 Installing the System...

  • Page 85: Troubleshooting, Testing, And Maintenance

    Troubleshooting, Testing, and Maintenance To avoid instrument damage, wait about 3 minutes after Caution: shutting down your system before you disconnect any interconnecting cables. Contents Topic Page Troubleshooting Performance tests 3-36 Maintenance procedures 3-47...

  • Page 86: Troubleshooting

    Troubleshooting You can easily correct many problems with your Prep Series system. If you cannot correct a condition, contact Waters Technical Service. Contacting Waters technical service North American customers who experience problems should contact Waters Technical Service at 800 252-4752. All others should call their local Waters subsidiary or Waters corporate headquarters in Milford, Massachusetts (USA).

  • Page 87: Troubleshooting Flowcharts

    - high valve and tubing to pressure shutdown transducer. not exceeded Mechanical problem Call Waters Technical Service. Pump shutting down, High flow rate during Decrease flow rate high pressure limit injection valve actuation during injection.
  • Page 88 (2414, 2410, and 410 purge port pressure of RI cell Detectors). Do not exceed exceeded 100 psi for any Waters RI detector. Replace detector flow cell if necessary (see detector operator’s guide). Peak retention times Incorrect pump head...

  • Page 89: Troubleshooting Flowcharts

    General PrepLC troubleshooting (Continued) Symptom Possible cause Corrective action System controller Screen saver feature Press any function key to screen is blank active display the screen. Increased system Normal condition. When To decrease system backpressure during the injector is in the backpressure, after injection using Inject position, the...
  • Page 90 Considerations When troubleshooting high system pressure, consider these: • Origin of the high pressure • Whether the pressure increase was gradual or sudden Location of pressure buildup To correct the high pressure condition, first isolate the part of the system in which the high pressure originates.

  • Page 91: High System Pressure

    Adjust Pressure Pressure pressure pressure reduced? reduced? transducer transducer Remove column. replace w/union. run system. Pressure Troubleshoot reduced? column Release injector outlet fitting Pressure Troubleshoot reduced? detector Release injector inlet fitting Troubleshoot Pressure injector reduced? Call Waters technical service Troubleshooting...
  • Page 92 Baseline noise If 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 following figure to determine what can cause an abnormal baseline. Troubleshooting, Testing, and Maintenance...

  • Page 93: Troubleshooting Chromatography

    Abnormal baseline troubleshooting Baseline abnormal Pump Troubleshoot pressure Noisy? pump constant? chromatography troubleshooting table Make sure Solvent correct Cycling? not mixing pressure filter properly is installed Allow Long-term Wrong column column to drift? equilibration? equilibrate Allow detector Detector not to warm up warmed up chromatography troubleshooting...
  • Page 94 Erratic or incorrect retention times Retention time changes Determine whether the retention times behave like this: • Change from run to run • Remain constant from run to run but extend beyond the allowable assay range Examining pressure fluctuations and changes When troubleshooting retention time problems, examine system pressure first.
  • Page 95 Mixing does not fluctuations environment apply to RI detectors. System Suggested actions: leaking? Column -Troubleshoot column contaminated? - Improve sample prep Troubleshoot pump: Isolate and - Seals troubleshoot - Check valves leak - Plunger Call Waters technical service Troubleshooting 3-11...
  • Page 96 Large pressure Isolate/ Is system drop associated troubleshoot leaking? with one pump leak head? Pump broken; Purge pump. troubleshoot pressure Still pump erratic? Call Waters technical service 3-12 Troubleshooting, Testing, and Maintenance...

  • Page 97: Poor Peak Resolution

    Poor peak resolution Before addressing problems with peak resolution, ensure that peaks are eluting at the correct retention time. The most common causes of poor peak resolution can also cause retention time problems. If peak retention time is correct, determine if the poor resolution occurs: •...
  • Page 98 (not column) clogged? Injector/column Use correct Continued on next page tubing diameter diameter tubing too large? Detector/column Use correct tubing diameter diameter tubing too large? Problem with Call Waters Troubleshoot injector? technical service injector 3-14 Troubleshooting, Testing, and Maintenance...
  • Page 99 Call Waters technical service Column Before using this troubleshooting tree, use those that appear earlier in the chapter to isolate the column as problem’s cause. Refer to the figure below to determine the possible cause of your column problem.

  • Page 100: Chromatography Troubleshooting

    Clean/replace Clean/replace Has plate column and column and count changed? determine plate determine plate count count Call Waters Technical Service Chromatography troubleshooting This section lists symptoms of chromatography problems, possible causes, and suggested corrective actions. 3-16 Troubleshooting, Testing, and Maintenance...
  • Page 101 Before using the table below, see “Troubleshooting steps” on page 3-2 isolate the cause of the chromatography symptom. Chromatography troubleshooting Symptom Possible cause Corrective action Erratic retention time Air in pump head Degas all solvents, prime pump, or check sparge rate. Malfunctioning pump Clean or replace pump check valves...
  • Page 102 Chromatography troubleshooting (Continued) Symptom Possible cause Corrective action Reproducibility errors Solvent not properly Degas or sparge degassed or sparged solvent. Incorrect chemistry Check chemistry. Incorrect integration Incorrect integration. Injector problem Troubleshoot injector. Baseline drift, rapid Column not Equilibrate column. equilibrated Detector not allowed to Allow detector to warm warm up...
  • Page 103 Chromatography troubleshooting (Continued) Symptom Possible cause Corrective action Baseline drift, slow Solvent contaminated Use fresh solvents. Decreased UV lamp Check lamp energy energy (detector documentation). Ambient temperature Stabilize operating fluctuations environment temperature enough to allow full equilibration. UV detector flow cell Check flow cell;...
  • Page 104 Chromatography troubleshooting (Continued) Symptom Possible cause Corrective action Baseline noise, Ambient temperature Stabilize operating long-term fluctuations environment (approximately 1 hour) temperature. cycling Integrator or recorder Check integrator or faulty recorder for excessive baseline noise. Straight baseline, no No pump flow Set pump flow rate.
  • Page 105 Chromatography troubleshooting (Continued) Symptom Possible cause Corrective action Baseline noise, random Air in detector Purge UV detector to remove air. Solvents not properly Sparge solvents. degassed Flow erratic, pump not Prime the pump; check primed for air in the pump, failing seals.
  • Page 106 Chromatography troubleshooting (Continued) Symptom Possible cause Corrective action Flat-topped peaks Detector not zeroed Zero detector baseline. Incorrect recorder input Adjust recorder input voltage voltage, or adjust detector output cable to proper position. Sensitivity too high Select a less sensitive detector range. Sample concentration Decrease sample or injection volume...

  • Page 107: Hardware Troubleshooting

    Replace power supply or missing fuse. Fan(s) not running Unit not turned on Turn unit on. Fan wiring or motor Call Waters Technical problem Service. Screen is blank Unit not turned on Turn unit on. Startup diagnostic test Power down and up failure again.
  • Page 108 Keypad is locked Unlock keypad on keypad PUMP SETUP screen. Keypad is broken Check keypad. CPU in Hold mode Call Waters Technical Service. Fluid system troubleshooting The table below addresses potential pump unit symptoms that can arise during operation. Pump troubleshooting Symptom...
  • Page 109 Pump troubleshooting (Continued) Symptom Possible cause Corrective action Pump leaks solvent Loose fitting Tighten leaking fitting. Salt crystals or debris Stop Flow; remove and in fitting disassemble fitting; rinse fitting components with water; reassemble fitting. Damaged fitting Stop Flow; remove and assembly disassemble fitting;...
  • Page 110 Pump troubleshooting (Continued) Symptom Possible cause Corrective action Erratic flow/pump Gas dissolved in mobile Sparge solvents. pulsations phase Air bubble in pump Prime pump to remove head bubble. Dirty check valve(s) Clean check valve(s). Faulty check valve(s) Replace check valve(s). Plugged solvent Clean or replace the reservoir filter...
  • Page 111 Waters autoinjector The table below lists autoinjector symptoms that can arise while operating a Waters autoinjector. Refer to the documentation that accompanies your autoinjector for additional troubleshooting information and service procedures. Replace both the needle and seal pack at the same time, because needle Tip: seal-pack sets are individually matched for optimal performance.
  • Page 112 Autoinjector troubleshooting (Continued) Symptom Possible cause Corrective action Reproducibility errors Syringe contains an air Remove bubble. bubble (usually seen at the top of the syringe) Leaks at the fluid Check for leakage at the tubing connections connections with the corner of a tissue, and tighten connection slightly if the tissue is moistened.
  • Page 113 1 Defective carousel Call Waters Technical reader Service. Detector troubleshooting Before using the troubleshooting tables in this section, use those that appear earlier in the chapter to identify the part of the system in which the problem originates.
  • Page 114 Replace fuse on lamp does not light power supply board. Lamp leads not Connect lamp leads. connected Replace lamp. Normal effects due to Call Waters Technical lamp aging Service. Bad lamp power supply board Unit will not calibrate Lamp aging Replace lamp.

  • Page 115: Software Troubleshooting

    Loss of sensitivity Foreign material in cell Clean cell and make sure solvent and column effluent are clean. Source LED needs Call Waters Technical replacement or is Service. misaligned Short term noise or drift Fluctuating ambient Stabilize environment. temperature Dirt in cell Clean cell.

  • Page 116: Replace With New Table

    To resume programming after a warning message, do one of these: • Press CLEAR. • Wait briefly until the message disappears. Operational warning messages Operational warning messages remind you to enter acceptable values and review your work. You must heed all warnings and take the appropriate corrective action. The table below lists the warning messages displayed on the controller.

  • Page 117: Illegal Vial Number

    Operational warning messages (Continued) Message Description Program Method Programming: Keyboard is locked while the SAVE Table Saved… function is storing the PROGRAM METHOD screen. This message is accompanied by an audible alarm. Check Programming: Since the Gradient, Event, and Corresponding Detector tables always run together (dictated by the Gradient table number), modifications made to the Gradient...

  • Page 118: First Vial Greater Than Last Vial

    To resume programming: Press CLEAR. Check the PUMP SETUP parameters. Make adjustments to the parameters. If the problem continues to occur, notify Waters Technical Service. System shutdown response When a shutdown occurs, the system responds as follows: • A message appears as: Shutdown Occurred - Reason:.....
  • Page 119 • The Hold output (on the controller’s rear panel) activates, signaling the connected instrument (for instance, the autoinjector) that the system is not ready for operation. • Gradient, Event, and Detector tables that were running abort. • The Autostart time and Table # fields reset to blank. •...

  • Page 120: Performance Tests

    To avoid damaging any equipment, wait about 3 minutes after Caution: shutting down your system before disconnecting any interconnecting cables. For problems you cannot resolve, contact Waters Technical Service for assistance. Self-diagnostics The Waters controller performs these self-diagnostic tests on startup: •...

  • Page 121: Extended Tests

    LCD display. Restart Restart the program by turning the power switch off and back on. If characters fail to appear a second time, 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.
  • Page 122 Counter test Verifies that the valves cannot switch to a 50/50 condition. If any tests fail during this procedure, contact Waters Technical Service. Tip: Tools The only tools required for the extended test routine are a jumper wire to short various controller rear panel terminals and a screwdriver.
  • Page 123 Rear panel terminals AC power connector AC Power Connector Pump Power Fuse Pump power fuse IEEE 488 CHART SWITCHES PRESSURE Screw Auxiliary +12 VAC Auxiliary +12 V Power Fuse terminals Screw Terminals RS232 power fuse System interface System Interface Connector PRESSURE connector CHART...
  • Page 124 To perform a stop flow input test: Attach a jumper wire from the Stop Flow switch on the rear panel to the Gnd terminal, also on the rear panel. Press ENTER. • If the test succeeds, the screen displays GOT STOP FLOW •...
  • Page 125 To perform an external switch (S1 to S4) output test: Attach a jumper wire from the S1 terminal to the INJ terminal on the rear panel. Press ENTER. The screen displays TEST PASSED TEST FAILED Press ENTER. Repeat steps 1 to 3 for the remaining switch terminals (S2 to S4). When you have tested all four external switches, the screen displays CONNECT HOLD TO INJECT If you want to perform the Hold Output test, do not press ENTER...
  • Page 126 A triangular (sawtooth) trace appears on the chart recorder if the test succeeds. Press ENTER to proceed to the next test. IEEE-488 address test This test verifies that the system is reading the current address. When the test begins, the current address appears on the screen. To perform an IEEE-488 address test: Change the position of any IEEE-488 address DIP switch on the back of the controller panel.
  • Page 127 Insert a jeweler’s screwdriver into the hole. Adjusting the transducer Turn the screwdriver slowly clockwise until the pressure display value reaches 0. Turn the screwdriver slowly counterclockwise until a small positive number appears. Solvent proportioning valve pair test This test lets you evaluate the system when you suspect a defective proportioning valve is causing erratic chromatographic results.
  • Page 128 Fill reservoirs C and D with solvent 2 (100% methanol with UV absorbing sample added). The concentration of UV absorbing sample used in solvent 2 should produce about 0.45 AUFS in this test. Flushing solvent lines Be sure to flush any residual solvents from the system. Adjusting the recorder To adjust the recorder: Set the detector to 0.5 AUFS.
  • Page 129 Gradient table values (Continued) Time Flow Curve 45.00 1.00 To perform a solvent proportioning valve pair test: Go to the OPERATE METHODS screen. Press the START RUN screen key. When the detector baseline is stable at 0%, do the following: Change the detector sensitivity to 0.1 AUFS.
  • Page 130 Test results with all valves working 3-46 Troubleshooting, Testing, and Maintenance...

  • Page 131: Maintenance Procedures

    Maintenance procedures This section includes maintenance procedures for the following components: • Fluid handling system • Rheodyne 7725i and 3725i injectors • Fuses To avoid damaging equipment, wait about 3 minutes after Caution: shutting down your system before disconnecting any interconnecting cables.

  • Page 132: Fluid Handling Unit Maintenance

    Tubing configuration in the column rack If you change fittings or tubing in the column rack, check for leaks before operating the unit. Fluid handling unit maintenance Observe safe laboratory practices when handling solvents. Warning: Refer to the Material Safety Data Sheet for the solvents in use. This section describes the maintenance or repair procedures for the fluid handling unit.
  • Page 133 • Pump head removal • Pump seal replacement • Pump plunger replacement • Wash seal replacement Pressure transducer calibration test You must calibrate the pressure transducer to the system. To perform a pressure transducer calibration test: Disconnect the column from the flow path by turning the Purge valve on the column rack to PUMP Purge.
  • Page 134 Replace the cover screw in the left hole. Cleaning and replacing check valves These are three types of check valves in the Waters Prep system pump: • Inlet valves, located under the pump head •...
  • Page 135 Cleaning check valves Clean check valves by running a nonionic detergent solution or 6N HNO through the pump heads. Flush with copious amounts of water to remove residual detergent or acid. Disconnect the column from the flow path. If the pump outlet is connected Tip: directly to the column (for large-scale operation), disconnect the column at its inlet from the flow path.
  • Page 136 The figure below shows an exploded view of the inlet check valve assembly. Clean and replace worn or damaged parts. Inlet check valve assembly Pump head PUMP HEAD Housing seal HOUSING SEAL Retainer clip RETAINER CUP Sleeve SLEEVE Ball BALL Seat SEAT SEAL GUIDE...
  • Page 137 To reassemble inlet check valves: Position the retainer cup so that you can look down into it. Insert the sleeve into the retainer cup. Place the ball in the retainer cup. Place the seat guide over the ball with the shiny side of the seat facing the ball.
  • Page 138 Outlet check valve assembly OUTLET CHECK Outlet check valve housing VALVE HOUSING Seal guide SEAL GUIDE Retainer clip RETAINER CUP Sleeve SLEEVE Ball BALL Seat SEAT Seal housing SEAL HOUSING Pump head To protect the parts from contamination, use forceps or Caution: tweezers to handle the parts after cleaning them and when reassembling the outlet check valve.
  • Page 139 Place the ball in the seat. Lower the sleeve around the ball, placing it on the seat. Place the retainer over the ball and seat assembly. Center it within the pump head. Place the seal guide into the outlet check valve housing. Press it into place.
  • Page 140 Dual check valve assembly Outlet check valve housing Seat Outlet check valve housing Seat Ball Seal guide Seal guide Removing the pump head The figure below is an exploded diagram of a pump head. Pump head disassembly Plunger bearings Pump head Pump seal PUMP SEAL ALLEN SCREW...
  • Page 141 Start the pump, setting the flow rate to 0.1 mL/min. Run it until the indicator rod retracts fully into the pump head. The indicator rod must be fully retracted into the pump Caution: head. Otherwise, the plunger can sustain damage. Shut down the pump.
  • Page 142 To remove the head support assembly: Remove the four plunger support screws with a 9/64-inch hex-head wrench. Slide the head support assembly and indicator rod off the plunger. Removing the head support assembly Continue with “Replacing the pump plunger” on page 3-61 “Replacing Tip: the plunger wash seal”...
  • Page 143 Pry the seal out of the pump head with a small screwdriver. Do not scratch the surface of the pump head. Do not damage the seat or score surrounding surfaces Caution: when you remove the seal. Removing the pump seal Use the seal insertion tool to insert the seal in the pump head: Put the seal onto the tip of the insertion tool so that the open end of the seal (with the spring) faces out from the end of the tool.
  • Page 144 Slide the insertion tool with the seal into the guide and press to firmly seat it in the pump head. Remove the insertion tool and guide. Inspect the plunger for scoring that could impair the Caution: seal. Replacing the pump head seal Insertion tool Seal Guide...
  • Page 145 Replacing the pump plunger This procedure requires moderate strength and dexterity as well as a Tip: 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.
  • Page 146 Pry the piston cap out of the piston, using a wire whose end is formed into a small hook. Insert the hook behind the cap and pull it toward you. Exposed plunger and piston Insert the plunger insertion tool into the piston cavity. With one hand, force the inner part of the plunger insertion tool against the snap ring.
  • Page 147 Using the plunger insertion tool and snap-ring pliers to remove the plunger Snap-ring pliers Plunger insertion tool Pull the plunger straight out of the cavity. Removing the plunger Maintenance procedures 3-63...
  • Page 148 Reassembling the plunger To reassemble the plunger: Place the two halves of the ball retainer around the ball on the plunger. Slide the spring over the ball retainer. The spring holds the ball retainer together. Lubricate the end of the ball with a lithium-based grease like Lubriplate™.
  • Page 149 15. Insert the two hex-head screws. 16. Reconnect the plunger wash lines and, with a syringe, push solvent through the two pump heads until it exits the second pump head. This primes the plunger wash and lubricates the plunger before you run the pump.
  • Page 150 Mount the new wash seal on the end of the insertion tool with the smooth side of the seal flush as shown below. Wash seal insertion tool TP02050 Push the seal into the head support assembly, making sure it firmly seats.

  • Page 151: Replacing Fuses

    Push the O-ring into place on the retainer. Gently slide the pump head onto the plunger, ensuring the indicator rod is in the correct hole. 10. Insert the two hex-head screws, holding the pump head assembly in place, and alternately tighten them. 11.
  • Page 152 The table below lists the correct fuses for your operating voltage. Operating voltage ranges Nominal AC Voltage Fuse (Amp) voltage range ±10% ±10% ±10% ±10% To replace fuses: Make sure the instrument is connected to the electrical power supply. Pry open the power connector cover on the back of the unit, next to the power cord.
  • Page 153 connector, pin end first. You can insert the holder into the connector in either orientation. Auxiliary +12 VAC fuse The 12-VAC fuse protects the AUX +12 VAC terminal on the controller rear panel from excessive current loads. If this fuse is open, no power is available from this terminal.
  • Page 154 Pump power fuse The pump power fuse protects the pump from excessive current loads. If this fuse is open, no power is available at the pump. To replace the power pump fuse: Shut down the controller and remove the power cord from its rear-panel connector.

  • Page 155: Maintaining Rheodyne Manual Injectors

    0.5-A fuse ATTENTION CAUTION DO NOT REMOVE CABLE WHILE UNIT IS POWERED CONNECT TO 4000 CONTROLLER ONLY 0.5-A fuse 0.5A FUSE To replace the 0.5-A fuse: Insert a small flat-blade screwdriver into the fuse holder for the 0.5-A fuse. Turn the screwdriver to release the fuse holder. Slide the holder with the fuse out from the rear panel.
  • Page 156 • Fixing rotor seal leakage Refer to the figure “Rheodyne 7725i injector: exploded view” on page 3-73 each procedure. Tightening the needle seal The needle seal, a PTFE sleeve in the rotor seal, may not seal correctly around a needle that is smaller than average. A poor seal results in a loss of accuracy in sample loading.
  • Page 157 Pull the position sensing switch out of the stop ring. Insert a new position sensing switch. Reassemble the injector according to the instructions in “Replacing the rotor seal” on page 3-74. Rheodyne 7725i injector: exploded view Handle screw Handle Knob Set screws (2) Needle guide Pressure adjusting screws...
  • Page 158 Fixing rotor seal leakage If you see liquid leak between the stator and stator ring, tighten the pressure adjusting screw. If you see it leak from the needle port or vent tube, replace the rotor seal. To tighten the pressure adjusting screw: Locate the pressure adjusting screw on the injector shaft (see the figure “Rheodyne 7725i injector: exploded view”...
  • Page 159 When replacing the rotor seal, always check the ceramic stator face for chips or cracks. If you find damage, replace it. Refer to the figure “Rheodyne 7725i injector: exploded view” on page 3-73 this procedure. To replace the rotor seal: Leave the injector attached to the front panel of the pump, and leave the knob on.
  • Page 160 Orient the rotor seal as shown below, with rotor seal slots facing the stator. Rotor seal orientation (viewed from the stator) Rotor pin Rotor Pin Notch Notch Replace the stator ring so the pin in the 60° stop ring enters the mating hole in the stator ring.

  • Page 161: Warning Symbols

    Safety Advisories Waters instruments display hazard symbols designed to alert you to the hidden dangers of operating and maintaining the instruments. Their corresponding user guides also include the hazard symbols, with accompanying text statements describing the hazards and telling you how to avoid them.

  • Page 162: A Safety Advisories

    Heed all warnings when you install, repair, and operate Waters instruments. Waters assumes no liability for the failure of those who install, repair, or operate its instruments to comply with any safety precaution.

  • Page 163: Specific Warnings

    The following warnings can appear in the user manuals of particular instruments and on labels affixed to them or their component parts. Burst warning This warning applies to Waters instruments fitted with nonmetallic tubing. Pressurized nonmetallic, or polymer, tubing can burst. Warning: Observe these precautions when working around such tubing: •...
  • Page 164 Also ensure a gas-fail connection is connected to the LC system so that the LC solvent flow stops if the nitrogen supply fails. Mass spectrometer shock hazard This warning applies to all Waters mass spectrometers. To avoid electric shock, do not remove the mass spectrometer’s Warning: protective panels.

  • Page 165: Caution Symbol

    Biohazard warning This warning applies to Waters instruments that can be used to process material that might contain biohazards: substances that contain biological agents capable of producing harmful effects in humans. Waters instruments and software can be used to analyze or...

  • Page 166: Warnings That Apply To All Waters Instruments

    Warnings that apply to all Waters instruments When operating this device, follow standard quality control procedures and the equipment guidelines in this section. Attention: Changes or modifications to this unit not expressly approved by the party responsible for compliance could void the user’s authority to operate the equipment.
  • Page 167 • Keine Schläuche verwenden, die stark geknickt oder überbeansprucht sind. • Nichtmetallische Schläuche nicht für Tetrahydrofuran (THF) oder konzentrierte Salpeter- oder Schwefelsäure verwenden. • Durch Methylenchlorid und Dimethylsulfoxid können nichtmetallische Schläuche quellen; dadurch wird der Berstdruck des Schlauches erheblich reduziert. Warnings that apply to all Waters instruments...
  • Page 168 Attenzione: fare attenzione quando si utilizzano tubi in materiale polimerico sotto pressione: • Indossare sempre occhiali da lavoro protettivi nei pressi di tubi di polimero pressurizzati. • Spegnere tutte le fiamme vive nell'ambiente circostante. • Non utilizzare tubi eccessivamente logorati o piegati. •...
  • Page 169 농축 질산 또는 황산과 함께 사용하지 마십시오. • 염화 메틸렌(Methylene chloride) 및 디메틸술폭시드(Dimethyl sulfoxide)는 비금속 튜브를 부풀려 튜브의 파열 압력을 크게 감소시킬 수 있으므로 유의하십시오. 警告：圧力のかかったポリマーチューブを扱うときは、注意してください。 • 加圧されたポリマーチューブの付近では、必ず保護メガネを着用してください。 • 近くにある火を消してください。 • 著しく変形した、または折れ曲がったチューブは使用しないでください。 • 非金属チューブには、テトラヒドロフラン(THF)や高濃度の硝酸または硫酸などを流 さないでください。 • 塩化メチレンやジメチルスルホキシドは、非金属チューブの膨張を引き起こす場合が あり、その場合、チューブは極めて低い圧力で破裂します。 Warnings that apply to all Waters instruments...
  • Page 170 Warning: The user shall be made aware that if the equipment is used in a manner not specified by the manufacturer, the protection provided by the equipment may be impaired. Attention: L’utilisateur doit être informé que si le matériel est utilisé d’une façon non spécifiée par le fabricant, la protection assurée par le matériel risque d’être défectueuses.
  • Page 171 警告 : 為了避免火災， 更換保險絲時， 請使用與儀器保險絲蓋旁面板上所印刷之相同類 型與規格的保險絲。 警告 : 为了避免火灾，应更换与仪器保险丝盖旁边面板上印刷的类型和规格相同的 保险丝。 경고: 화재의 위험을 막으려면 기기 퓨즈 커버에 가까운 패널에 인쇄된 것과 동일한 타입 및 정격의 제품으로 퓨즈를 교체하십시오. 警告 : 火災予防のために、ヒューズ交換では機器ヒューズカバー脇のパネルに記 載されているタイプおよび定格のヒューズをご使用ください。 Warnings that apply to all Waters instruments A-11...

  • Page 172: Electrical And Handling Symbols

    Electrical and handling symbols Electrical symbols These 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 Frame, or chassis, terminal Fuse Recycle symbol: Do not dispose in municipal waste.

  • Page 173: Handling Symbols

    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! Fragile! Use no hooks! Electrical and handling symbols A-13...
  • Page 174 A-14 Safety Advisories...

  • Page 175: B Specifications

    Specifications This appendix contains specifications for the following: • Operational • Electrical • Environmental Operational specifications Item Specification Number of solvents One to four Modes of operation Gradient, isocratic, and flow programming Operating flow Programmable from 1 to 150 mL/min in range 0.01-increments (500-µL heads) and from 4 to 300 mL/min in 0.01-increments (1000-µL heads).
  • Page 176 Operational specifications (Continued) Item Specification Program storage Storage for sets of 15 tables (Gradient, Event, and Detector), with up to 15 steps per table. Storage for a time-based multimethod program with up to 48 individual steps, linking sets of tables. EEPROM stores setup parameters and tables and preserves memory indefinitely following power loss or extended shutdown.
  • Page 177 • Exceeding high pressure limit • Below low pressure limit • Abort input • Startup condition Used to communicate with Hold input on Waters autoinjectors or other compatible inputs to prevent further injections. Chart output Two terminals (+, –) for recording pump flow rate...
  • Page 178 Environmental specifications Item Specification Temperature Operating range: 4 to 38 °C (39 to 100 °F) Storage range: 0 to 50 °C (32 to 122 °F) Humidity Operating range: 20 to 90% relative humidity Storage range: 0 to 90% relative humidity (noncondensing) Solvent Compatible with solvents consistent with materials of...

  • Page 179: C Spare Parts

    Spare Parts This appendix lists the spare parts that are recommended for customer installation. Use the number in the Recommended Stock column as a guide to the quantity of each item to keep on hand. Common parts Item Recommended stock Part number Valve, 3-way purge 700001309...

  • Page 180: Gradient

    150-mL configuration Item Recommended stock Part number 150-mL Conversion Kit 0 205000135 Inlet/Outlet Check WAT037495 Valve Rebuild Kit Inlet Check Valve WAT033325 Assembly Outlet Check Valve WAT033326 Assembly Plunger Assembly 700002123 Plunger Seal Kit WAT037490 Gradient Proportioning WAT082823 Valve Assembly 300-mL configuration Item Recommended stock...
  • Page 181 Solvent Considerations Contents Topic Page Clean solvent Solvent miscibility How to use miscibility numbers (M-numbers) Buffered solvents Solvent head height Solvent viscosity Solvent degassing Solvent degassing methods...

  • Page 182: D Solvent Considerations

    If the filter becomes plugged, clean or replace it. If the Waters Prep system is not used for several weeks, flush the system (outlet line, inlet lines, and check valves) with filtered, distilled water containing 10% methanol or acetonitrile.

  • Page 183: Solvent Miscibility

    Solvent miscibility Before changing from one solvent to another, see the table below to determine the miscibility of the solvents being used. The following considerations apply when changing solvents: • Changes involving two miscible solvents are made directly. Changes involving two solvents which are not totally miscible (for example, from hexane to water) require an intermediate solvent (such as methanol or THF).
  • Page 184 Physical properties of solvents (Continued) Boiling Miscibility Polarity Viscosity Wavelength Solvent Point °C Number index CP, 20 °C Cutoffs (nm) (1 atm) Methylene 0.44 39.8 chloride Ethylene 0.79 83.5 — chloride Butyl alcohol 3.00 117.7 — — Butanol 3.01 177.7 —...

  • Page 185: How To Use Miscibility Numbers (M-Numbers

    Physical properties of solvents (Continued) Boiling Miscibility Polarity Viscosity Wavelength Solvent Point °C Number index CP, 20 °C Cutoffs (nm) (1 atm) Dimethylsul- 2.24 189.0 — foxide Methanol 0.60 64.7 Formamide 3.76 210.5 — Water C.00 100.0 — — a. Adapted from Godfrey, Norman B., Solvent Selection via Miscibility Number, CHEMTECH, 359-363 (1972).

  • Page 186: Buffered Solvents

    Store the pump in 10% methanol/water during the shutdown. Solvent head height The Waters Prep system is flexible in allowing you where to position the solvent reservoirs. Ideally, the reservoirs should be positioned approximately level with the pump heads, particularly at flow rates of 2.0 mL/min or less.

  • Page 187: Solvent Degassing

    water and methanol produces twice the pressure of either water or methanol alone. If the extent to which the pressure changes will affect the analysis is not known, monitor the pressure during the run using the controller’s Chart output provided for this purpose (select %A or %B). Solvent degassing Mobile phase difficulties account for 70% or more of all problems in liquid chromatography.

  • Page 188: Solvent Degassing Methods

    Helium sparging combines the convenience of short initial degassing time required, ease of maintaining the solvent condition during operation, and complete control within the framework of the Waters Prep systems. 1. S. R. Bakalyar, M. B. T. Bradley, R. Hoganen, Journal of Chromatography, 158 (1978) 277.
  • Page 189 The degassing operation should be as efficient as possible. To remove the gas as quickly as possible, be aware of the following considerations: • Helium sparging gives stable baselines and better sensitivity in a fluorescence detector, and prevents the reabsorption of atmospheric gases.
  • Page 190 D-10 Solvent Considerations...

  • Page 191: Index

    Column switching valve burst warning Column troubleshooting 3-15 Composition Must Sum to 100% message 3-33 Cabling Connection ports 1-13 AC power 2-15 Connector types 1-10 IEEE-488 2-15 Contacting Waters Technical Service PowerLine 2-17 Can’t Save Table Currently Executing Controller message 3-32 Index-1...
  • Page 192 Empower IEEE-488 cabling 2-15 2-18 IEEE-488 addresses 2-18 ENTER key 1-17 powerup/power down sequence Entering values 1-17 2-18 equipment guidelines Waters 746 RS-232 cabling 2-20 Erratic retention times 3-10 Waters 845/860 IEEE-488 cabling Error messages 2-15 clearing 1-17 Degassing solvents reproducibility 3-18...
  • Page 193 2-15 2-17 pump leaks 3-25 data system powerup sequence pump not running 3-24 2-19 pump squeak 3-26 Empower cabling 2-15 Fraction collectors, Waters 1-13 IEEE-488 address, setting 2-18 Front panel 1-16 – 1-19 PowerLine controller cabling 2-17 controller keys 1-18 –...
  • Page 194 replacing 3-51 3-53 pump seal replacement 3-58 – retainer cup 3-51 replacing +5 A fuse 3-70 – 3-71 Inlet port connection 2-38 replacing auxiliary power fuse 3-69 Installing replacing operating voltage fuse plastic tubing fittings 2-25 3-67 Rheodyne injectors with Delta-Prep mass spectrometer shock hazard 2-40 Messages...
  • Page 195 Plunger wash fluid handling unit Rack, column 1-12 seal replacement 3-65 3-67 – Radial-Pak cartridges 1-14 Potentiometer, adjusting 3-49 Random baseline noise 3-21 Power Up screen, leaving 1-16 Rapid baseline drift 3-18 Powering down Rear panel connections, terminal strip sequence 2-19 3-39 system...
  • Page 196 A-12 digital input 1-10 handling A-13 ground terminal 1-11 warning hold 1-10 System modules, Waters Prep Series open collector 1-10 Slow baseline drift 3-19 System pressure, reference point Small-scale flow path 1-12 System shutdown response 3-34 Small-scale sample injection valve...
  • Page 197 Delta-Prep system poor peak resolution 3-13 Waters Prep Series Tubing, installing plastic fittings 2-26 choosing controller 1-22 powering down 1-19 powering up 1-14 UV detectors system modules 1-13 lamp not lit 3-30 Waters PrepLC system. See PrepLC troubleshooting 3-30 system Index-7...
  • Page 198 Waters Technical Service, contacting Workstations Empower 2-15 MassLynx 2-15 Index-8...

This manual is also suitable for:

Hplc

Table of Contents