WATERS CORPORATION 2424 Operator'S Manual Download Page 111

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4-1

Maintaining the Detector

Contents:

Topic

Page

Contacting Waters technical service

4-2

Maintenance considerations

4-2

Replacing the lamp cartridge

4-3

Replacing the nebulizer

4-6

Cleaning the nebulizer ultrasonically

4-9

Cleaning the drift tube

4-12

Servicing the vapor trap

4-13

Replacing fuses

4-14

Cleaning the instrument’s exterior

4-15

Summary of Contents for 2424

Page 2: ...rs 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 dama...

Page 3: ...encounter in this document or to suggest ideas for otherwise improving it Please help us better understand what you expect from our documentation so that we can continuously improve its accuracy and u...

Page 4: ...esentative for guidance When you develop methods follow the Protocol for the Adoption of Analytical Methods in the Clinical Chemistry Laboratory American Journal of Medical Technology 44 1 pages 30 37...

Page 5: ...rs Intended use of the 2424 ELS detector Waters designed the 2424 ELS detector to analyze and monitor many compounds Symbol Definition Confirms that a manufactured product complies with all applicable...

Page 6: ...mal normal and above normal levels of a compound Ensure that QC sample results fall within an acceptable range and evaluate precision from day to day and run to run Data collected when QC samples are...

Page 7: ...vii 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 8: ...viii...

Page 9: ...i ISM classification vi ISM Classification ISM Group 1 Class B vi EC Authorized Representative vii 1 2424 ELS Detector Optics Principles 1 1 Principles of evaporative light scattering detection 1 2 Ov...

Page 10: ...sions 2 5 Power requirements 2 6 Gas requirements 2 7 Making the gas supply connection 2 7 Venting the exhaust hose 2 8 Connecting to the electricity source 2 11 Installing the nebulizer assembly 2 12...

Page 11: ...ng to start a run 3 15 Primary and secondary functions 3 15 Setting up a run 3 17 Setting the nebulizer and drift tube temperature 3 18 Setting the gain and gas pressure 3 19 Setting the column heater...

Page 12: ...method 3 39 Viewing events within a method 3 39 Resetting a method 3 39 Clearing events 3 40 Conserving lamp life 3 41 Changing chromatographic conditions 3 43 Shutting down the detector 3 44 Periodi...

Page 13: ...eypad diagnostic functions 5 8 Gas and temperature control diagnostic functions 5 10 Sample and reference energy diagnostic function 5 12 Generate Test Peaks diagnostic function 5 13 General troublesh...

Page 14: ...Drift tube temperature 6 10 Selecting the optimum temperature 6 10 A Safety Advisories A 1 Warning symbols A 2 Task specific hazard warnings A 2 Specific warnings A 3 Caution symbol A 5 Warnings that...

Page 15: ...he 2424 ELS detector effectively you must understand the principles that underlie operation of the detector s optics and electronics Contents Topic Page Principles of evaporative light scattering dete...

Page 16: ...molecules natural product extracts and libraries food products and related materials For detecting compounds that exhibit little to no UV Vis response and do not ionize well for mass spectrometry the...

Page 17: ...heat to evaporate the solvent Conversely low gas flow produces large droplets requiring more heat to evaporate the solvent Desolvation In the desolvation region the mobile phase evaporates leaving dri...

Page 18: ...sizes exhibit different angular distributions of the scattered light and particles whose sizes and shapes vary have different light scattering cross sections In general larger particles scatter more...

Page 19: ...ng type depends on the size of the particles going through the light beam The ratio of particle diameter D to the incident wavelength or defines the type of scattering that results Rayleigh scattering...

Page 20: ...cks linearity over wide concentration ranges When you use the detector for assays you may need to experiment with a variety of best fits using linear quadratic and log log responses for the compounds...

Page 21: ...Detector description The detection of a sample peak occurs as follows 1 Eluent from the column flows into the nebulizer where a steady supply of gas converts it into a fine aerosol Carefully controll...

Page 22: ...g gaseous effluent is vented Signal processing and noise calculations Power source fluctuations can introduce noise in the detector output and be a major source of noise at high signal levels To offse...

Page 23: ...oard It also interfaces between the Preamplifier board and the CPU board CPU board Contains the microprocessor serial RS232 and Ethernet communications battery backed nonvolatile RAM in which the user...

Page 24: ...can interact The chamber contains these components Two light traps Reference photodiode To prevent the solvent and analyte from condensing on the chamber walls or optical surfaces the chamber is heat...

Page 25: ...tile samples Drift Tube You can set the drift tube heater up to 100 C to evaporate any residual solvent RTD resistance temperature detector sensors provide temperature feedback to the heater control t...

Page 26: ...s response varies with energy throughput If the lamp energy is degraded peak response degrades accordingly If lamp intensity diminishes peak response decreases and noise increases During normal operat...

Page 27: ...Contemporary Instrumental Analysis Simon Schuster Prentice Hall Inc New Jersey 2000 G D Christian Analytical Chemistry Sixth Edition John Wiley Sons Inc New York 2003 TP02730 EXHAUST 15cm 6 inch CLEAR...

Page 28: ...hromatography Edited by E Yeung J Wiley Sons New York 1986 B A Bidlingmeyer Practical HPLC Methodology and Applications Wiley Sons NY 1992 U Neue HPLC Columns Theory Technology and Practice Wiley VCH...

Page 29: ...Guiochon Use of light scattering as a detector principle in liquid chromatography J Chromatogr 265 1 1983 G Guiochon A Moysan and C Holley Influence of various parameters on the response factors of t...

Page 30: ...1 16 2424 ELS Detector Optics Principles...

Page 31: ...y 2 3 Making the gas supply connection 2 7 Venting the exhaust hose 2 8 Connecting to the electricity source 2 11 Installing the nebulizer assembly 2 12 Connecting the siphon drain tubing 2 14 Connect...

Page 32: ...ate laboratory instruments and computer controlled devices and also how to handle solvents Make Signal Connections to Start installation procedure Installation complete Select appropriate site Unpack...

Page 33: ...the shipping cartons for future transport or shipment If you discover any damage or discrepancy when you inspect the contents of the cartons immediately contact the shipping agent and your local Wate...

Page 34: ...ector the amount of weight stacked on top of it should not exceed 18 kg 40 pounds Installation site requirements Parameter Requirement Operating temperature range 4 to 30 C 39 2 to 86 F avoid direct e...

Page 35: ...nnections are located Gas supply 450 to 690 kPa 4 5 to 6 9 bar 65 to 100 psi at the regulator of dry oil free filtered nitrogen or zero grade oil free filtered air Ventilation Locate near fume hood or...

Page 36: ...s distributor Power off and unplug the detector before performing any maintenance on the instrument Connect all components of the HPLC system to a common ground Warning For continued protection agains...

Page 37: ...the gas supply connection 1 Cut the 6 mm tubing squarely that is perpendicular to the tubing s horizontal axis Warning Do not use gases that are not inert In particular avoid those that would allow th...

Page 38: ...vided in the startup kit If you are using the system with an external filter first connect the gas source to the filter and then connect the filter to the back of the unit Venting the exhaust hose To...

Page 39: ...se to an evacuation source but do not apply a vacuum Caution Failure to use the vapor trap could result in too strong a vacuum which could adversely affect the vapor flow through the drift tube This c...

Page 40: ...ings on the vapor trap bottle Vapor trap bottle and exhaust hose Warning Inhalation risk Do not allow detector exhaust to enter the laboratory atmosphere Caution To avoid excessive electronic noise do...

Page 41: ...2 kPa 0 bar 0 03 psi between the detector and the laboratory exhaust system Exhaust system flow example Connecting to the electricity source The 2424 ELS detector requires a separate grounded electri...

Page 42: ...ord to a suitable wall outlet 4 Do not turn the detector on at this time Installing the nebulizer assembly Waters offers two nebulizers for the 2424 ELS detector a low flow for flow rates from 50 to 5...

Page 43: ...the nebulization chamber The quick disconnect tubing fitting will be at the twelve o clock position Installing the nebulizer 6 Push the nebulizer into the nebulization chamber and turn it clockwise u...

Page 44: ...ase Omitting this step delays satisfactory detector performance Routing the siphon drain tubing down the front of the detector Required materials Front siphon drain tubing in startup kit Hose clamp to...

Page 45: ...the end of the tubing is not immersed in the collected liquid Routing the siphon drain tubing to the rear of the detector Tip The rear siphon drain tubing is intended for use with the optional Waters...

Page 46: ...he hole in the siphon drain tubing bracket and align the screw and bracket with the hole that you removed the cover screw from 3 Using a Phillips screwdriver secure the bracket to the front left side...

Page 47: ...6 Route the other end of the rear siphon drain tubing through the opening in the rear left corner of the detector tray 7 Attach the convoluted tubing to the rear siphon drain tubing using the plastic...

Page 48: ...f the unit in the event of a leak Required materials Tubing not supplied Sharp knife not supplied To connect the drip tray 1 Cut a length of tubing sufficient to reach between the drip tray and the wa...

Page 49: ...d exhausts it as gas vapor Do not allow solvent flow to continue if no gas flow is present Required materials Sample inlet tubing assembly 5 16 inch open end wrench To connect a column or second detec...

Page 50: ...king signal connections Tip Connect the detector to other HPLC system components through an Ethernet connection The figure on page 2 6 shows the rear panel locations of the connectors used to operate...

Page 51: ...or or chart recorder Yes Yes Install Ethernet cable No Connect to Ethernet bus Start signal connection Signal connection complete Install event and I O cable s No Connect event inputs or outputs Insta...

Page 52: ...Ethernet cable This cable is contained in the startup kit Single Waters instrument connection Multiple Waters instrument connections In a system configuration with many Waters Ethernet instruments an...

Page 53: ...se a network switch for multiple Ethernet instruments Use of a network hub in place of a network switch is not supported Multiple Waters Ethernet instrument connections Connecting to a Waters MassLynx...

Page 54: ...ent system configurations Tip For pinout connections to the detector see page 2 26 Detector inject start connections Inject start output source Inject start input connection on the 2424 ELS detector c...

Page 55: ...the detector to other instruments use the two analog out event in I O connectors and their corresponding pin outs on the rear panel This section describes signal connections between the detector s re...

Page 56: ...time clock to start Lamp on Enables and disables the lamp When the input is active the lamp is on Chart mark in Adds a chart mark at 10 of full scale to either or both analog output channels Signal Ou...

Page 57: ...e column heater temperature or gas pressure and is programmable Output voltage range 0 1 to 2 1 VDC fixed maximum data rate is 10 Hz Stop flow Stops the flow to the chromatographic system when a low i...

Page 58: ...shown in the following table and figure Warning Fire and explosion hazard Failure to connect the stop flow output could cause the detector to flood 1 2 3 4 5 6 7 8 9 10 Inject Start In Inject Start In...

Page 59: ...lliance separations module Alliance separations module connector B 2424 ELS detector connector I Pin 4 stop flow red Pin 6 stop flow red Pin 5 stop flow black Pin 7 stop flow black 1 2 3 4 5 6 7 8 9 1...

Page 60: ...output connections to a chart recorder Chart recorder connectors 2424 ELS detector connector I Pen 1 Pin 1 signal out red Pen 1 Pin 2 signal out black Tip For this connection do not use the cable shie...

Page 61: ...injector Inject start signal from a contact closure signal with each injection Auto zero signal to adjust the zero offset of the detector each time the injector makes an injection Each time the detec...

Page 62: ...ctor Inject start connections to an injector pulse duration 0 to 10 seconds 2424 ELS detector connector II Injector connector Pin 1 inject start in red Two spade lug terminal connectors both cables ma...

Page 63: ...Connecting the Waters column heater module The detector can control one Waters column heater module through the EXT port on the rear panel of the detector The port is a standard 9 pin D type connecto...

Page 64: ...2 34 Setting up the Detector...

Page 65: ...igating the user interface 3 13 Preparing to start a run 3 15 Setting up a run 3 17 Configuring the detector 3 26 Operating the detector 3 30 Programming methods and events 3 34 Conserving lamp life 3...

Page 66: ...As part of a MassLynx System Use the detector configured with a MassLynx system To configure the detector with a MassLynx system follow the instructions in the MassLynx documentation to set the param...

Page 67: ...ts are coded for use only by Waters Service Engineers for troubleshooting When initialization is complete the detector displays the Home screen see page 3 7 and page 3 13 Detector Home screen Tip For...

Page 68: ...ge 5 14 for hardware related causes of confidence tests failure during startup and their corrective actions Using the display The detector employs a 128 64 bitmap graphic display and a 24 key membrane...

Page 69: ...following table Detector Home and Message screen icons Icon or field Icon field name Function Gain Selects the gain setting Regular field PSI Gas pressure Displays the current gas pressure and allows...

Page 70: ...asterisk which indicates current conditions are not stored as a method Remote control Indicates that the detector is controlled by a data system and displays a remote control icon 0 00 Run time Displ...

Page 71: ...Configure DIAG Diagnostics and TRACE Primary function keys Chart Mark Auto Zero Run Stop and Next Primary function keys take effect immediately with no further entry required Secondary function keys R...

Page 72: ...sired item then press Enter For the number 10 select 0 and then press Enter To go to the end of a choice list press For entries numbered 11 or 12 press the or key to scroll to the desired item on the...

Page 73: ...p Starts or stops pauses the run clock The elapsed time appears near the lower right hand corner of the Home screen Reset Resets the detector run clock to zero minutes and returns the detector to init...

Page 74: ...Displays the list of options for creating and clearing timed and threshold events and storing retrieving and resetting methods DIAG Displays the list of diagnostic routines CONFIG Displays the first C...

Page 75: ...te of the lamp is indicated by an icon on the Home screen 4 See 0 9 above System Info Displays system information including software version checksum and instrument serial number 5 See 0 9 above Lock...

Page 76: ...ctive field CE Clears an editing change and returns the contents of a field to its previous value Sets the value to a unique word for some fields For example in the voltage offset diagnostic you may e...

Page 77: ...through the list and then press Enter Tips If you know the number corresponding to the desired choice you can press that number without pressing Enter first The and keys do not increase or decrease nu...

Page 78: ...3 of 5 4 of 5 and 5 of 5 Secondary functions of the Home screen Auto zero on inject and gain enable keypad and event in for auto zero and chart mark Light scattering Home screen Data rate and time con...

Page 79: ...the gain factor from 1 to 1000 Each gain setting has a linear relationship with the actual light scattering signal Gas pressure Gas pressure is controlled at the nebulizer by a pressure regulator Thi...

Page 80: ...Baseline Maintain Baseline Nebulizer heater level Heating Cool Off Heater level 0 to 100 or Cool Cool Drift tube heater set temp C Off 5 to 100 C Off Drift tube heater alarm band C 5 to 25 C 20 C Col...

Page 81: ...o program several other parameters depending on the functions you want to perform during a run See page 3 15 for function descriptions fields screen number type of function display units allowable ran...

Page 82: ...eheating of the sample solution to the set heater power level via a resistive heat wrap that surrounds the nebulizer tube From the Nebulizer and Drift Tube Temperature Control Home screen you control...

Page 83: ...scale sensitivity of the detector by defining the gain factor from 1 to 1000 Each gain setting relates linearly with the actual light scattering signal The gas pressure setting monitors the condition...

Page 84: ...Home screen appears Gain and Gas Pressure Home screen 2 Enter the gain amount in the Gain field Once you enter a gain amount the photomultiplier tube PMT is activated 3 To turn off the PMT enter 0 in...

Page 85: ...view any changes in the current field Resetting the stop flow output switch A dedicated switch stop flow becomes active when a heater gas flow or lamp failure occurs Once the cause of the error is co...

Page 86: ...n on a particular section of the trace To display the Scale parameters 1 Press Scale 2 Press Next to display T2 starting time The default is 0 3 Press Next again to display LSU1 starting or low light...

Page 87: ...0 screen shown above T1 is changed to 5 T2 is changed to 0 LSU1 and LSU2 remain as auto scaled Scaled trace for 5 minutes changing T1 to 5 The following screen shows a 30 minute scaled trace similar t...

Page 88: ...r 80 Hz To set the data rate 1 From the Home screen press Next The data rate and time constant function screen appears Data rate and time constant function screen 2 Use Enter and the numeric keypad or...

Page 89: ...t full scale value defines the maximum output voltage value that will be used to represent the units full scale value For example using the default values the units full scale value of 2000 is represe...

Page 90: ...he On Inject check box at the start of a run the detector either evaluates the auto zero adjustment based on no signal zero or it resets the auto zero adjustment to zero Configuring the detector Press...

Page 91: ...to select the appropriate entry Chart mark You can specify the input to create a chart mark on signal output To determine the response of the channel use the chart mark function High Create chart mar...

Page 92: ...configuration screen When the active state is Off the stop flow output is normally On until a stop flow error condition occurs At that point the stop flow output is changed to the Off state Requireme...

Page 93: ...cting the type of nebulizer You use the fourth configuration screen to select the appropriate nebulizer for your flow rate range High flow 0 3 to 3 mL minute Low flow 05 to 5 mL minute Setting the dis...

Page 94: ...ng help The detector offers limited context sensitive Help When you press press Shift HOME from a point in the program with which a Help screen is associated the screen appears If Help is unavailable...

Page 95: ...rt of the ideal gain values appears on screen The report is based on a computation that maximizes use of one half the range of the electronics so a 2 margin accommodates any variations in signal inten...

Page 96: ...optimization Gain optimized chromatograph Recommended method development approach You should use a method with two timed event changes to optimize this chromatogram The first gain setting change could...

Page 97: ...ctor s Instrument Method Editor Under Empower control the method is downloaded to the detector when you make an injection or if the method is set up Once you program the method into the detector or Em...

Page 98: ...Separations Module When the run is completed press Run Stop Reset The detector displays a recommended LSU FS value and a table of gain values Programming methods and events Overview of methods The det...

Page 99: ...are deactivated when power is restored On startup you always see an asterisk inside the method icon on the Home screen When the detector is operating under remote control the remote icon appears Prog...

Page 100: ...enter the time To advance to the set field Events choice list press 5 Press Enter again to display the choice list or if you know the event number press the number for the event you are programming 6...

Page 101: ...ied threshold the switch is set as shown in the table below You can program the switch parameters listed in the table To define the pulse period or the frequency of a wave see page 3 26 To program a t...

Page 102: ...arameter you are programming Storing a method A method consists of all programmable parameters on the Home and associated screens as well as timed and threshold events You can store the current method...

Page 103: ...Method choice list the method number you specified appears within the method number icon Viewing events within a method To view timed and threshold events that make up a stored method 1 Retrieve the m...

Page 104: ...s Tip To prevent losing the current conditions before you clear the method store them in one of the available storage slots When you clear the storage slots you can restore the previous conditions 4 P...

Page 105: ...h it while allowing the detector to remain powered on You can do this in three ways Manually By programming a timed event By programming the lamp itself via the external contact closure Tip If you are...

Page 106: ...front panel 1 Press Lamp press Shift 1 The lamp control screen displays this information The amount of time in hours and minutes the lamp has been ignited since the most recent startup The total time...

Page 107: ...on using a timed event See page 3 27 for more information on programming the lamp through the external contact closure Changing chromatographic conditions Requirement When the detector is plumbed to t...

Page 108: ...tes to drain the evaporation tube and detection chamber 5 Stop the gas flow 6 Power off the power to the detector Tips The last set of selected parameters is retained in memory and becomes the default...

Page 109: ...aintenance Tip To avoid damaging the column remove it before you remove the mobile phase from the fluid path 1 Set the drift tube temperature at the appropriate desolvation temperature setting Tip 50...

Page 110: ...3 46 Operating the Detector...

Page 111: ...hnical service 4 2 Maintenance considerations 4 2 Replacing the lamp cartridge 4 3 Replacing the nebulizer 4 6 Cleaning the nebulizer ultrasonically 4 9 Cleaning the drift tube 4 12 Servicing the vapo...

Page 112: ...Problem symptom s Nebulizer and drift tube temperatures Heater set points and levels Flow rate Filter setting System operating pressure Gas pressure Solvent s System configuration other components Fo...

Page 113: ...To prevent injury always observe Good Laboratory Practices when you handle solvents change tubing or operate the system Know the physical and chemical properties of the solvents you use See the Materi...

Page 114: ...s with the fan running and then remove the left front panel cover 3 Using a Phillips screwdriver completely loosen the two captive screws and pull the assembly out slightly to relieve stress on the la...

Page 115: ...nplug the detector before detaching the lamp power connector from the detector Caution To avoid damaging the detector s electronics power off and unplug the detector before detaching the lamp power co...

Page 116: ...t the power cable from the rear panel 3 Remove the left hand front panel cover Warning To avoid burn injuries do not touch the nebulizer until its temperature cools to less than 30 C as displayed on t...

Page 117: ...zer as follows a Use a 5 16 inch wrench to loosen the compression screw that holds the inlet tubing in place b Remove the solvent inlet tubing from nebulizer 5 Push in the quick disconnect tubing fitt...

Page 118: ...nect tubing fitting is at the twelve o clock position Then remove it from the nebulization chamber 7 Remove the packing ring from the old nebulizer and slide it onto the new nebulizer If the old packi...

Page 119: ...Push the nebulizer into the nebulization chamber and turn it clockwise until it snaps into place 10 Insert the gas inlet tubing into the quick disconnect tubing fitting on the right side of the nebul...

Page 120: ...n screw that holds the inlet tubing in place b Remove the solvent inlet tubing from the nebulizer Warning To avoid burn injuries do not touch the nebulizer until its temperature cools to less than 30...

Page 121: ...n and turn the nebulizer counterclockwise so that the quick disconnect tubing fitting is at the twelve o clock position Then remove it from the nebulization chamber 7 Remove the packing ring from the...

Page 122: ...the gas inlet tubing into the quick disconnect tubing fitting on the right side of the nebulizer and place the nebulizer in a dry beaker so that it stands up 14 Run gas at 410 kPa 4 1 bar 60 psi for 5...

Page 123: ...semble the detector for operation 6 Reset the system to operating conditions and evaluate chromatography Servicing the vapor trap To service the vapor trap 1 Unscrew the vapor trap bottle from the cov...

Page 124: ...ng loaded fuse holder which fits above the power entry module on the rear panel of the detector With minimum pressure withdraw the spring loaded fuse holder 3 Remove and discard the fuses 4 Make sure...

Page 125: ...leaning the instrument s exterior 4 15 5 Reconnect the power cord to the power entry module Cleaning the instrument s exterior Use a soft cloth dampened with water to clean the outside of the detector...

Page 126: ...4 16 Maintaining the Detector...

Page 127: ...pparent detector problem may actually originate with the chromatography or other system instruments If you isolate a general chromatography problem see Chromatography troubleshooting on page 5 21 If y...

Page 128: ...essage screen Errors described on this screen can be catastrophic in nature preventing further operation of the detector suspending the light scattering display and halting output The error messages c...

Page 129: ...to the number on the detector keypad Menu items that display further choices are accompanied by Diagnostic functions Diagnostic function Description Reset flow diags Resets all diagnostic functions to...

Page 130: ...ings You can disable all active sticky diagnostics by pressing DIAG 1 Reset Flow Diags If no sticky diagnostics are active the wrench icon does not appear in the home screen Lamp display keypad Lists...

Page 131: ...ice personnel can access service diagnostics To exit any diagnostic when completed press DIAG to return to the diagnostics menu or HOME to return to the Home screen Running the Auto Gain diagnostic fu...

Page 132: ...Auto Gain diagnostic press Enter Input and output diagnostic functions Use the input and output diagnostic functions for these purposes To view and reset the sample signal s auto zero value To fix es...

Page 133: ...fixed but the values can be set independently The valid range of voltages is 2000 mV for both channels The voltage is driven on the selected channel Detector Out or Auxiliary Out Monitoring contact cl...

Page 134: ...e lamp display and keypad diagnostic functions press DIAG 5 Change Lamp diagnostic function Use the Change Lamp diagnostic function to enter the serial number and installation date of a new lamp To us...

Page 135: ...p use information To use the Lamp History function From the Lamp display keypad menu press 2 Lamp history The Lamp History diagnostic screen appears Lamp History diagnostic screen Test Keypad diagnost...

Page 136: ...To use the Test Display function 1 From the Lamp display keypad menu press 4 Test display The display fills from top to bottom and right to left It then returns to the Lamp display keypad menu If the...

Page 137: ...nostic function you can control the gas pressure regulator and gas solenoid valve independently The diagnostic screen displays the state of the gas pressure switch and the value of the pressure transd...

Page 138: ...r 0 in the set point field Sample and reference energy diagnostic function With the sample and reference energy diagnostic function you view raw sample signal and reference energy information and you...

Page 139: ...g This section suggests possible causes of errors and recommends troubleshooting actions Keep in mind that the source of apparent detector problems can actually be the chromatography or it can involve...

Page 140: ...n heater module to detector Detector inoperative Fuse blown Check that the front panel display is operational if it is not check or replace the AC rear panel fuse No power at outlet Check the outlet b...

Page 141: ...tray Properly attach and route the waste tube Keypad not functioning Keypad defective 1 Power off and then power on the detector 2 Run the keypad diagnostic see page 5 9 3 If the problem persists cal...

Page 142: ...ilure sample ADC Lamp or PMT signal too low Weak lamp or bad alignment 1 Replace the lamp see page 5 8 2 Power the detector off and then on 3 If the problem persists call Waters Technical Service see...

Page 143: ...leak in bench Light entering optics bench 1 Power off and then power on the detector 2 If the problem persists call Waters Technical Service see page 4 2 System not normalized Run diagnostic Memory wa...

Page 144: ...ter failure short circuit Cable or connector short Problem with personality board 1 Power off and then power on the detector 2 If the problem persists call Waters Technical Service see page 4 2 Column...

Page 145: ...Heater failure short circuit Cable or connector short Problem with personality board 1 Power off and then power on the detector 2 If the problem persists call Waters Technical Service see page 4 2 Dr...

Page 146: ...d then power on the detector 2 If the problem persists call Waters Technical Service see page 4 2 Nebulizer heater temperature probe failure The heater s temperature probe is not connected or has a lo...

Page 147: ...exhibits symptoms not addressed in one of the tables refer to General troubleshooting on page 5 13 If you need further help contact Waters Technical Service Optics heater rose above its set temperatur...

Page 148: ...hase mixing problem causing improper evaporation Correct mobile phase composition Use high quality HPLC water and organic solvents Drift tube temperature not optimized correctly Recalculate temperatur...

Page 149: ...aust trap Check for kinks in exhaust line or empty condensate flask Column leaking silica or packing material Replace column and flush it thoroughly before connecting it to the detector Air trapped in...

Page 150: ...ctor is making a gurgling sound Detector exhaust too strong Move exhaust hose further away from vacuum See the figure Exhaust system flow example on page 2 11 Drift tube not heating Tube temperature n...

Page 151: ...ix the error then restart the pump Flow interrupted or obstructed Check mobile phase level in reservoirs Check flow throughout system Make sure mobile phase inlet filter is clean Leak Check system for...

Page 152: ...ase Peak should be seen immediately Detector output signal not zeroed Press the Auto Zero key No gain set Set gain see page 3 19 Detector exhaust too strong Move exhaust hose further away from vacuum...

Page 153: ...phase is degrading or that the column is contaminated Change early in a series of runs and tend to become constant or fall within range after a few minutes which can indicate that the column was not...

Page 154: ...ed retention times Air bubble in pump head Prime pump to remove bubble Malfunctioning pump check valve s Clean replace or rebuild pump check valve s Broken pump plunger Replace the plunger Reduced ret...

Page 155: ...cy is poor throughout the chromatogram post column band broadening or loss of column efficiency can be the cause If only one peak in a chromatogram is badly shaped the peak component may be interactin...

Page 156: ...connection between the detector and the recorder Auto zero detector baseline Check cables between unit and recorder No sample injected Check injector Leak in solvent path Check fittings and drip tray...

Page 157: ...ults troubleshooting Symptom Possible cause Corrective action Decreased peak height Leak in injector Troubleshoot injector Degraded contaminated or improperly prepared sample Use fresh sample Column c...

Page 158: ...too low Increase drift tube temperature see page 3 18 Drift tube temperature too high Decrease drift tube temperature see page 3 18 Nebulizer temperature too high Decrease nebulizer power level see p...

Page 159: ...is chapter presents information on detector performance common solvent problems solvent selection degassing a solvent Warning To avoid chemical hazards always observe safe laboratory practices when ha...

Page 160: ...atment If the sample contains any particulate matter filter it through a 0 2 m or 0 45 m filter before injection Column treatment The chromatographic column contains microparticles to separate the com...

Page 161: ...ilter before use The total organic carbon reading should be as low as possible 5 ppb Buffer compatibility The detector cannot be used with nonvolatile solvents such as salt buffer solutions Volatile m...

Page 162: ...solvents The following table lists the properties for some common chromatographic solvents Warning THF contaminants peroxides can explode when concentrated or evaporated to dryness Warning Do not use...

Page 163: ...alcohol 32 4 at 20 C 82 26 12 Isopropyl myristate 1 at 20 C 192 6 164 Methanol 97 at 20 C 64 7 11 Methyl t butyl ether 240 at 20 C 55 2 28 Methyl ethyl ketone 74 at 20 C 79 64 9 Methyl isobutyl keton...

Page 164: ...H range Boiling Point C Acids Acetic Acid 4 75 9 25 116 00 Carbonic Acid 6 37 7 63 Formic Acid 3 75 10 25 100 70 Trifuoroacetic Acid 0 30 13 70 71 80 Bases Ammonia 9 25 4 75 33 35 Ethylamine 10 81 3 1...

Page 165: ...n These methods may be used individually or in combination Vacuum ultrasound followed by sparging is the most effective technique for most solvents Sparging Sparging removes gases from solution by dis...

Page 166: ...o remove dissolved gas quickly consider the following Vacuum degassing The longer a solvent is exposed to the vacuum the more dissolved gases are removed Two factors affect the amount of time the solv...

Page 167: ...ause less gas is consumed and a better sensitivity is achieved However at some point this benefit is offset by an increase in baseline noise from the inefficient nebulization of the eluent resulting i...

Page 168: ...izer gas flow rate However the evaporator temperature must be high enough to evaporate the solvent and sufficiently dry the particle plume without adversely affecting the sample If the evaporator temp...

Page 169: ...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 170: ...ks include burn injuries electric shocks ultraviolet radiation exposures and others When the following symbols appear in a manual s narratives or procedures their accompanying text identifies the spec...

Page 171: ...ction Extinguish all nearby flames Do not use tubing that is or has been stressed or kinked Do not expose nonmetallic tubing to incompatible compounds like tetrahydrofuran THF and nitric or sulfuric a...

Page 172: ...al surfaces of the mass spectrometer when the instrument is in Operate mode To avoid non lethal electric shock make sure the instrument is in Standby mode before touching areas marked with this high v...

Page 173: ...When operating this device follow standard quality control procedures and the equipment guidelines in this section Warning Waters instruments can be used to analyze or process potentially hazardous s...

Page 174: ...er Modifikationen an dem Ger t ohne die ausdr ckliche Genehmigung der f r die ordnungsgem e Funktionst chtigkeit verantwortlichen Personen kann zum Entzug der Bedienungsbefugnis des Systems f hren Avv...

Page 175: ...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 176: ...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 177: ...Warnings that apply to all Waters instruments A 9 Nonmetallic Tetrahydrofuran THF Methylene chloride Dimethyl sulfoxide THF...

Page 178: ...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 179: ...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 180: ...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 181: ...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 182: ...A 14 Safety Advisories...

Page 183: ...ght 14 7 kg 32 5 pounds Environmental specifications Attribute Specification Operating temperature 4 to 30 C 39 2 to 86 F Operating humidity 20 to 95 noncondensing Shipping and storage temperature 30...

Page 184: ...outlet c Pollution Degree 2 A measure of pollution on electrical circuits which may produce a reduction of dielectric strength or surface resistivity Degree 2 refers only to normally nonconductive pol...

Page 185: ...5 A Current carry 1 2 A Temperature control Nebulizer heater power 0 to 100 Nebulizer cooler Cooling Off Drift tube heater Ambient to 100 C 212 F a Signal and Auxiliary b Inject Start Lamp On Chart M...

Page 186: ...B 4 Specifications...

Page 187: ...biohazard warning A 4 burst warning A 3 C calibration photomultiplier tube 1 8 PMT 1 8 Cancel key 3 12 caution symbol A 5 CE key 3 12 changing contrast 3 11 data rate 3 13 filter time constant 3 13 sc...

Page 188: ...sting 3 29 changing 3 11 function 3 29 key 3 11 controller board 1 9 controlling from Empower system 3 2 from MassLynx system 3 2 CPU board 1 9 current method conditions 3 13 3 34 3 40 D damage report...

Page 189: ...6 event inputs auto zero 3 27 chart mark 3 27 configuring 3 27 default 3 28 inject start 3 27 lamp 3 28 exhaust venting requirements 2 9 external analog data collection device connecting 2 30 F failu...

Page 190: ...7 inject start connection 2 24 generating 2 27 signal 2 24 injection trigger signals connecting 2 31 input and output connectors 2 26 installing fuses 2 6 major steps 2 2 network guidelines 2 23 proce...

Page 191: ...maintenance considerations 4 2 mass spectrometer shock hazard A 4 MassLynx system control 3 2 maximum voltage outputs function 3 13 method active 3 39 choice list 3 10 current conditions 3 13 initial...

Page 192: ...ed event 3 35 threshold timed event 3 35 peak identification 5 31 resolution 5 29 troubleshooting 5 30 photomultiplier tube calibration 1 8 physical specifications B 1 plus minus key 3 12 PMT calibrat...

Page 193: ...te 3 24 drift tube temperature 3 18 filter time constant 3 24 gain 3 19 gas pressure 3 19 nebulizer temperature 3 18 pulse periods 3 28 switch output 3 25 setting up a run 3 17 shift icon 3 5 Shift ke...

Page 194: ...s 3 34 3 41 auxiliary switch parameters 3 35 clearing 3 40 deleting 3 36 description 3 35 gas pressure parameters 3 35 lamp parameters 3 35 parameters auto zero 3 35 chart mark 3 35 programming 3 34 3...

Page 195: ...22 V vacuum degassing 6 7 6 8 vapor trap servicing 4 13 viewing events within a method 3 39 voltage offset function 3 13 W warm up time 3 3 warning symbols A 2 A 5 Waters Technical Service contacting...

Page 196: ...Index 10...

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Summary of Contents for 2424

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WATERS CORPORATION 2424, Operator'S Manual, Page: 111 / 196

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Summary of Contents for 2424

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