Home

ICS-Series Photodiode Array Detector Manual

1. gt AVERTISSEMENT Signale une situation de danger potentiel qui si elle n est pas vit e pourrait entrainer des blessures mineures mod r es Egalement utilis pour signaler une situation ou une pratique qui pourrait MISE EN GARDE gravement endommager l instrument mais qui n entrainera pas de blessures gt Warnhinweise in Deutsch Bedeutet unmittelbare Gefahr MiBachtung kann zum Tod oder schwerwiegenden Verletzungen f hren gt ACHTUNG Bedeutet eine m gliche Gefahrdung MiBachtung kann zum Tod oder schwerwiegenden Verletzungen f hren gt WARNUNG Bedeutet eine m gliche Gef hrdung MiBachtung kann zu kleineren oder mittelschweren Verletzungen f hren Wird auch verwendet wenn eine Situation zu schweren Sch den am Ger t f hren kann jedoch VORSICHT keine Verletzungsgefahr besteht gt Informational messages also appear throughout this manual These are labeled NOTE and are in bold type NOTE NOTES call attention to certain information They alert users to an unexpected result of an action suggest how to optimize instrument performance etc 8 Doc 065378 01 1 12 1 Introduction 1 4 2 1 4 3 Safety Labels These symbols appear on the Dionex PDA or on Dionex PDA labels Alternating current Primary protective conductor terminal Secondary protective conductor terminal Power supply is on Power supply is off Indicates a potential hazard Refer to this operator
2. 125 B 10 2 Selecting Configuration Properties 127 B 11 Starting the Chromeleon 128 C Reordering Information 131 Doc 065378 01 1 12 Dionex PDA Operator s Manual vi Doc 065378 01 1 12 1 e Introduction 1 1 Detector Overview Figure 1 1 Thermo Scientific Dionex ICS Series Photodiode Array Detector The Thermo Scientific Dionex ICS Series Photodiode Array Detector Dionex PDA P N 074114 is an optical chromatography detector capable of measuring absorbance signals and absorbance spectra from 190 to 800 nm The Dionex PDA can be used with the following Thermo Scientific Dionex systems the ICS 5000 analytical systems only ICS 2100 ICS 1600 ICS 1100 and ICS 900 as well as some legacy systems The Dionex PDA can be used in numerous laboratory environments for routine analysis as well as for sophisticated research tasks A deuterium lamp optimizes the UV range 190 to 380 nm and a tungsten lamp optimizes the visible range 380 to 800 nm When using the Dionex PDA up to five single wavelengths 2D chromatograms can be collected without the necessity for collecting 3D data Collecting individual wavelengths instead of the spectra offers two advantages it eliminates the need to perform signal extractions for analyses that do not require spectral data and it conserves disk space Doc 065378 01 1
3. 22 116 Default settings 42 Output 116 Analog output range 22 Analytes unknown 46 Audit Trail 13 59 Automated control 29 Index Average 43 Definition 53 Guidelines for selecting 53 Avertissement icon 8 B Backpressure 56 Increase 55 Backpressure line 76 Installation 115 Bandwidth 43 Definition 46 Guidelines for selecting 46 Setting is too narrow 76 Baseline drift 43 48 Causes 95 Reducing 48 Troubleshooting 78 79 Baseline noise 43 Causes 82 93 95 Reducing 44 46 48 50 85 Relationship to rise time 44 Bolts 10 32 115 Bunch width 43 Definition 51 Guidelines for selecting 51 C Cable USB 122 Installation 120 122 Calibration wavelength 2 82 88 Caution icon 7 Cells 15 16 43 Air bubble prevention 75 115 Air bubble removal 93 Doc 065378 01 1 12 Index 1 Dionex PDA Operator s Manual Backpressure line 76 Backpressure line installation 115 Chemical compatibility 43 Cleaning procedure 93 Contaminants 76 Heat exchangers 17 19 91 108 Illustration 17 19 114 Installing 113 Leaks 13 Path length 107 109 Specifications 107 Stains inside 97 Chromeleon 6 8 2 3D Data Acquisition license 4 30 Audit Trail 13 59 87 Automated control 41 Commands dialog box 40 Connecting to 35 Diagnostic procedures 87 Direct control 38 Direct control mode 38 Installation 119 Overview of automated control 41 Panel tabs
4. Eee beret ee 105 A 2 Physicalisii led le iL e Re ES SOR EET HER 105 Environmental 105 Ad Detector Ben a ee eae 106 A5 Blow Cells ioca eer ee a eat Slane 107 AS Standard Flow Cell EE 107 A 5 2 Semi Micro Flow 107 A 5 3 Semi Preparative Flow Cell 108 Ap Heat Exchangers ENEE EEN s En 108 B INStANAUON aat 111 B 1 Facilities Requirements 111 B 2 Unpacking jes eos bee ede ld 112 Installing the Flow 113 B 4 Connecting the Waste Lime 116 B 5 Connecting the Analog Outputs Optional 116 B 6 Connecting the Relays TTLs Optional 117 B 7 Connecting to the Chromeleon 118 B 7 1 Before You Begin 118 B 8 B 7 2 Chromeleon 7 Starting the Instrument Controller Service 119 B 7 3 Chromeleon 6 8 Starting the 119 B 7 4 Connecting the USB Cable 120 Connecting the Power Cord 123 Doc 065378 01 1 12 Contents B 9 Installing the USB Device Drivers 124 B 10 Configuring the Dionex PDA in Chromeleon 125 B 10 1 Using the USB Auto Configuration 7
5. 1 Te UV VIS 2 Figure 3 2 Example Dionex PDA Control Panel in Chromeleon 6 8 d Verify that the Connected check box is selected If it is not click the box to connect the Dionex PDA to Chromeleon 6 8 NOTE After starting Chromeleon 6 8 and connecting to the Control panel the Connected LED on the detector s status bar is blue 36 Doc 065378 01 1 12 3 e Operation and Maintenance 3 1 4 Turn On the Lamps To turn on the lamps click UV Lamp and Vis Lamp on the Chromeleon 7 ePanel see Figure 3 1 or the Chromeleon 6 8 Control panel see Figure 3 2 When a detector lamp is turned on for the first time after the detector power is turned on wavelength calibration is performed automatically Calibration starts shortly after the lamp is ignited 3 2 System Equilibration Before you can begin using the Dionex PDA for sample analysis the chromatography system must be equilibrated To equilibrate the system perform the following tasks Pump the starting solvent through the entire system until the system is free of any other liquid composition Heat or cool all temperature controlled devices for example a column compartment to the temperature required for the application Set the detector wavelength s and turn on the lamp s Calibrate the wavelength s Monitor the pump pressure and verify that the reading is correct for the application and is stable Monitor the detector signal and verify that the
6. A 5 Flow Cells A 5 1 Standard Flow Cell Cell Body PEEK or 316 stainless steel Volume and PEEK cell 13 uL volume 10 mm 0 394 in path length Optical Path Stainless steel cell 13 uL volume 10 mm 0 394 in path length Length Maximum PEEK cell 2 MPa 300 psi Operating Stainless steel cell 3 MPa 500 psi Pressure Chemical Do not use bases stronger than 0 1 M these solutions will Compatibility etch the fused silica windows of the flow cell e Do not use normal phase or chlorinated solvents with the PEEK flow cell these solutions will damage the cell Do not use low pH solutions with the stainless steel flow cell these solutions may cause corrosion contamination and metal leaching A 5 2 Semi Micro Flow Cell Cell Body PEEK or 316 stainless steel Volume and PEEK cell 3 1 uL volume 9 mm 0 35 in path length Optical Path Stainless steel cell 3 1 uL volume 9 mm 0 35 in path length Length Maximum PEEK cell 2 MPa 300 psi Operating Stainless steel cell 3 MPa 500 psi Pressure Doc 065378 01 1 12 107 Dionex PDA Operator s Manual Chemical Compatibility e Do not use bases stronger than 0 1 M these solutions will etch the fused silica windows of the flow cell e Do not use normal phase or chlorinated solvents with the PEEK flow cell these solutions will damage the cell e Do not use low pH solutions with the stainless steel flow cell these solutions may cause corrosion contamina
7. BW Reference bandwidth For example the following parameters are VALID Wavelength 190 to 500 nm Reference wavelength 450 nm Reference bandwidth 50 nm These parameters are valid because 190 to 500 nm is a range of lt 310 nm and 450 nm 25 nm 50 of 50 nm 475 nm which is less than 500 nm The following parameters are NOT VALID Wavelength 190 to 600 nm Reference wavelength 750 nm Reference bandwidth 50 nm These parameters are invalid because 190 to 600 nm is a range of more than 310 nm also 750 nm 25 nm 50 of 50 nm 775 nm which is greater than 600 nm Acquisition On for 3DFIELD rejected no 3D Data Acquisition license found To troubleshoot Chromeleon cannot perform digital data acquisition of a 3D data field unless the software includes the 3D Data Acquisition license Contact Thermo Fisher Scientific if you want to order this option Doc 065378 01 1 12 63 Dionex PDA Operator s Manual A Autozero is already in progress To troubleshoot This message appears if you select Autozero in the Chromeleon 7 Command window or the Chromeleon 6 8 Commands dialog box when the autozero routine is already in progress Allow the autozero routine to continue running until completion Calibration is running To troubleshoot This message appears if you attempt to issue a command or select a parameter while a calibration procedure is in progress Wait until the procedure finishes
8. Detach ePanel Smart Startup 25 Smart Shutdown Default Pump UV Vis Audit Startup Queue Device ICS 3000 PDA 10907 panon Uv VIS 2 Connected SC UV_VIS_3 226 B Uv VIS 4 trol onitols ess Uv VIS 5 Lao Pump 1 Pressure e e ax Pump 2 Pressure ius UV Lamp Uv VIS 1 Data Collection 10 00 s 200 200 Rise Time 2 00 gt 0 ro A Step Ave 200 200 Uv 1 210 nm gt d 4004 F 400 Uv2 254 S 21 6004 600 272 Si uva 5202 3 93 wee min Uv5 600nm gt 1 1 1000 0 0 2 5 5 0 7 5 10 0 Date Time Fetention Device Message Figure B 9 Example Dionex PDA ePanel in Chromeleon 7 Chromeleon 6 8 Client 1 Click Start on the Windows taskbar and select All Programs gt Chromeleon gt Chromeleon To display the Chromeleon 6 8 panel tabset click View gt Default Panel Tabset or click the corresponding toolbar button 128 065378 01 1 12 B Installation 3 display the Dionex PDA Control panel see Figure B 10 select the Dionex PDA tab on the panel tabset The Control panel provides access to Dionex PDA functions as well as detailed status and diagnostics information System_1 5 Home Sequence Coria Status Autosamgler Gradent Pumps Detector System_1 CMADLERT 2 34 00 AM Chromaleon server version 6 80 SP1 Build 2234 RC 3 started s
9. In Chromeleon 7 In Chromeleon 6 8 Create a sequence and specify Create a sequence and specify the instrument method files to use for program files to use for each each injection injection Load the sequence into the queue Load the sequence into the batch Start the queue Start the batch NOTE Before creating a program review Section 3 4 for a description of the detector parameters how they interact with each other and guidelines for their selection 3 3 3 Stand Alone Analog Operation This section describes limited stand alone operation of the Dionex PDA when the detector is not interfaced to a PC running Chromeleon In stand alone operation TTL inputs on the Dionex PDA rear panel can be used to trigger autozero or to turn the lamps on and off All other detector parameters remain at their factory default settings and cannot be changed Doc 065378 01 1 12 41 Dionex PDA Operator s Manual Factory Default Settings The Dionex PDA outputs four analog signals at all times even when the detector is not interfaced to a computer Data is presented at the analog output channels whenever the detector power is on A chart recorder or other voltage measuring device can be used to monitor the channels When the Dionex PDA power is first turned on the analog output settings are at the factory defaults listed in the table below Channel Single Bandwidth Reference Full Scale Offset Wavelength W
10. Lift the Dionex PDA by the side or bottom only the front cover of the IMPORTANT es detector snaps into place and must not be used for lifting Do not turn on the Dionex PDA unless it is at room temperature 4 to 40 C 40 to 104 F If you move the detector from a cold environment to a warm environment wait at least 1 hour for condensation to evaporate before turning on the power e Unpack all items in the Dionex PDA Ship Kit P N 060977 and check them against the packing list If there are any discrepancies notify Thermo Fisher Scientific immediately NOTE Keep the original shipping container and all packing material These will be needed if the detector is ever shipped or is moved to a new location 112 Doc 065378 01 1 12 B Installation B 3 Installing the Flow Cell Do not touch the cell windows If you touch a window clean it with IMPORTANT isopropyl alcohol IPA and a clean lens tissue Do not use a PEEK flow cell with normal phase or chlorinated IMPORTANT solvents these solvents will damage the cell Do not use a stainless steel flow cell with low pH solutions these IMPORTANT oes e solutions may cause corrosion contamination and metal leaching 1 Grasp the Dionex PDA front cover by the sides and pull straight off to remove 2 Remove the flow cell cover from the inside front panel see Figure 2 3 3 Standard or semi micro cell Remove the tubing bracket from the lamp cover
11. ZC Cell Inlet Tubing Reducing Union Fitting 1 p 3 Ech Heat Exchangers Spring Clip Figure 2 6 Semi Micro Flow Cell Assembly Semi Micro Cell Component PEEK Cell SST Cell Inlet tubing 0 12 mm 0 005 in ID P N 063897 N A Outlet tubing 0 38 mm 0 015 in ID P N 057304 N A Inlet tubing 0 12 mm 0 005 in ID N A P N 063903 Outlet tubing 0 25 mm 0 010 in ID N A P N 051650 Reducing union fitting P N 055903 P N 055902 18 Doc 065378 01 1 12 Ze Description Semi Preparative Flow Cell The semi preparative flow cell assembly see Figure 2 7 is available in PEEK only The cell is designed for use with semi preparative flow applications and flow rates of 5 0 to 100 0 mL min The 0 4 mm path length minimizes detector absorbance for concentrated peaks Cell Outlet Tubing 0 51 mm 0 020 in ID Union Fitting Qu P N 042627 Sus x P N 042855 Union Fitting o P N 042627 Cell Inlet Tubing 0 51 0 020 in ID P N 042855 Handle N LRL ga Spring Clip Flow Cell Figure 2 7 Semi Preparative Flow Cell Assembly Doc 065378 01 1 12 19 Dionex PDA Operator s Manual 2 4 Electronics Do not attempt to access the Dionex PDA electronics The components on the PC boards cannot be serviced by the user If servicing is required it must be performed by qualified personnel and CAUTION appropriate e
12. gt WARNUNG Connection of relay loads and their power sources to the TTL outputs will damage the TTL output stage If the relay load can source more than 200 mA at 5V or higher it may damage the Data Processing board SHOCK AND FIRE HAZARD Inputs and outputs are not rated for connection to an AC power main DO NOT CONNECT TO 100 115 220 230 OR 240 VAC POWER SOURCES FIRE OR ELECTROCUTION MAY RESULT DANGER D ELECTROCUTION D INCENDIE Le module d alimentation lectrique fonctionne aux potentiels du secteur Faites effectuer toutes les r parations par un personnel qualifi STROMSCHLAG UND BRANDGEFAHR Das Modul zur Stromversorgung wird mit Netzspannung beirieben Der Service darf nur von qualifiziertem Personal durchgef hrt werden The Dionex PDA Ship Kit P N 060977 includes a 12 pin connector P N 923686 for relay and TTL connections see Figure B 4 To attach individual wires and twisted pairs to the connectors strip the end of the wire s insert into the connector and tighten the locking screw s with a small screwdriver P N 046985 NOTE A twisted wire assembly P N 043598 is available as an option RELAY OUT TTL TTL IN TTL OUT GND 1 2 lla 2l41 2 3 4 1 2 12 34 5 6 7 8 9 101112 Figure B 4 Relay and TTL Connector Doc 065378 01 1 12 117 Dionex PDA Operator s Manual The table below describes the pin assignments for the relay and TTL connector Re
13. Click the Instruments Category Bar on the Console c Onthe Navigation Pane click the instrument that includes the detector The ePanel Set for the instrument appears in the Console Work Area d To display the detector ePanel click the UV Vis tab on the ePanel Set see Figure 3 1 e Verify that the Connected check box is selected If it is not click the box to connect the Dionex PDA to Chromeleon 7 NOTE After starting Chromeleon 7 and connecting to the ePanel the Connected LED on the detector s status bar is blue 34 Doc 065378 01 1 12 3 e Operation and Maintenance Help 5 lt Autogenerated gt Monitor Baseline 82 Command Detach ePanel Smart Startup 9 Smart Shutdown Defaut Pump UV Vis Audit Startup Queue Device ICS 3000 PDA 20005 2000 Uv VIS 2 connectes UV VIS 3 mem Uv VIS 4 t ontrols ead UV VIS 5 Lus Pump 1 Pressure Ka GES Pump 2 Pressure We UVLamp Ve Lamp aog ___iuvvs 1 S Data Collection 10 00 E 200 200 Rise Time 2 00 E 0 ro A Step Ave 200 200 RAA lead E E 2 7 400 7 400 uv2 254nm S 3 Si 6004 reng 272 Ej 0 994 nein min 600nm s 2000 T 1000 0 0 2 5 5 0 7 5 10 0 Date Device Message Figure 3 1 Example Dionex PDA ePanel in Chromeleon 7 3 1 3 Connect to t
14. Index 2 Doc 065378 01 1 12 Index DEUTERIUM UV LED LED is flashing 12 73 74 LED is lighted 12 70 Deuterium lamp 14 15 Calibration 80 Intensity 56 Lamp does not light 73 Maintenance 56 Output waning 76 Part number 131 Power supply 21 Replacing 98 Resetting the lamp age 87 See also Lamps Time in use 100 102 Time to stabilize 33 37 75 78 Diagnostic procedures 59 Chromeleon 87 PDA Moduleware 87 Dionex Technical Support 59 Direct control 29 Disk space 43 45 46 Conserving 1 46 Drain tube 22 116 E Electrical specifications 105 Electromagnetic interference EMI 20 Electronics 20 Electrostatic discharge ESD 20 ePanel Set 27 Equilibration system 75 Using the Smart Startup feature 38 Error messages 13 F Fan 21 68 Speed 21 Ferrule fittings 68 75 Part number 115 Filter paddle 14 15 Malfunction 77 80 Positions 15 Flow cells See Cells See Type of cell Front panel Illustration 11 LEDs described 13 Fuses 24 105 Part number 131 Replacing 103 G Gradient applications 26 53 Reference wavelength selection 48 79 Grating optical 14 15 H Heat exchangers 17 19 108 Operating pressure 108 Tubing connections 91 Volume 16 108 109 Holmium oxide filter 2 15 Filter paddle positions 15 Wavelength verification 15 Humidity operating 105 I ICS 3000 systems USB compatibility issues 121 ICS
15. To turn off the pump press and hold the power button for 2 seconds If the detector is not installed with a Dionex ICS 5000 or Dionex ICS 3000 system use the power button on the front of the Dionex PDA for routine on off control Check the status of the LEDs on the front of the detector The following LEDs should be lighted POWER DEUTERIUM UV and or TUNGSTEN VIS LED Wait 20 to 30 minutes for the lamps to stabilize For sensitive applications work or for detector validation allow at least 2 hours After installing a new lamp allow 8 to 24 hours Doc 065378 01 1 12 33 Dionex PDA Operator s Manual 3 1 2 Connect to the Chromeleon 7 Client 1 Start the Instrument Controller Service if it is not already running If the Chromeleon tray icon on the taskbar is crossed out in red the Instrument Controller Service is not running To start it right click the icon and select Start Chromeleon Instrument Controller The icon changes to gold b to indicate that the Instrument Controller Service is starting When the Instrument Controller Service is running idle the icon changes to gray E If the Chromeleon tray icon is not on the taskbar click Start gt All Programs Chromeleon 7 Services Manager to open the Services Manager and click Start Instrument Controller Start the Chromeleon 7 client a Click Start on the Windows taskbar and select All Programs gt Chromeleon 7 Chromeleon 7 b
16. running before making any changes Cannot change 3DFIELD parameters while data acquisition is running To troubleshoot This message appears if you attempt to select a parameter for the 3D field while data acquisition is in progress Wait until data acquisition is complete or stop the run and then change the parameters Cannot set manual parameters for the required operation because the DSP is not ready To troubleshoot This message appears if certain commands are issued before the DSP digital signal processor is ready to accept them Turn off the Dionex PDA power for 30 seconds and then turn it on again If the error message appears again contact Thermo Fisher Scientific for assistance 64 Doc 065378 01 1 12 4 Troubleshooting Can t execute calibration command during data acquisition Can t execute diagnostic command during data acquisition Can t execute x command during data acquisition To troubleshoot During data acquisition no other commands can be executed Wait until data acquisition is completed before attempting to issue any other command Command not executed because an Autozero command is already running To troubleshoot Wait until the autozero routine is completed before attempting to issue any other command Datais unavailable To troubleshoot This message appears if the Dionex PDA fails to respond when the computer attempts to communicate with the de
17. see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 66 Doc 065378 01 1 12 4 Troubleshooting b Select UV and then select LampIntensity The intensity reading should be above 10 million counts for a standard or semi preparative cell or above 3 million counts for a semi micro cell If the reading is acceptable resume normal operation If the reading is too low see Section 4 7 3 Ifthe error message appears again there may be a faulty connection to the filter wheel sensor Contact Thermo Fisher Scientific for assistance NOTE The Dionex PDA electronics cannot be serviced by users All repairs of the electronics components must be performed by Thermo Fisher Scientific personnel Invalid rise time Valid rise times at 20 Hz 0 05 0 1 0 2 0 5 A 1 0 and 2 0 To troubleshoot This message appears if you enter a rise time setting that is invalid for a data collection rate of 20 Hz Select a valid rise time Invalid step for the 3DFIELD Valid steps are 0 05 0 1 0 2 0 4 0 5 1 2 and 4 To troubleshoot This message appears if you enter an invalid step setting Chromeleon 7 or Chromeleon 6 8 automatically selects the step value that is the inverse of the data collection rate see Step Chromeleon 6 8 only on page 52 In future accept the value selected by the software Only advanced users should override the step setting selected by IMPORTANT i Chromeleon Selecting
18. 0 megohm cm Organics TOC 10 ppb Iron Transition Metals ppb Pyrogens 0 03 Eu mL Particulates gt 0 2 um lt 1 units mL Colloids Silica 10 ppb Bacteria lt 1 cfu mL ron transition metal content not specified for ASTM Type I water Table B 1 ASTM Filtered Type Deionized Water Specifications for lon Chromatography e Optical detectors are sensitive to vibration Provide a sturdy vibration free workbench of a height that allows convenient access to the interior of the Dionex PDA e Allow at least 6 cm 2 4 in behind the Dionex PDA for power connections and ventilation Do not block air flow to the detector During operation room air must be inducted into the detector to cool the electronics and dissipate the heat generated by the lamps Doc 065378 01 1 12 111 Dionex PDA Operator s Manual e The Dionex PDA can be positioned in many locations within a system the options include Above a Dionex ICS 5000 Thermal Compartment Below a Thermo Scientific Dionex AS AP Autosampler On either side of an integrated system for example the Dionex ICS 2100 Ion Chromatography System e Optical detectors are sensitive to changes in temperature and light Protect the Dionex PDA the columns and all tubing connections from drafts Do not operate the Dionex PDA unless the front cover lamp cover and flow cell cover are in place B 2 Unpacking e Carefully remove the Dionex PDA from the shipping container
19. 01 1 12 97 Dionex PDA Operator s Manual 5 7 Replacing the Deuterium Lamp 1 2 3 gt gt 2 0 Stop the Chromeleon instrument controller or server Press the power button on the front of the Dionex PDA to turn off the power Turn off the main power switch on the Dionex PDA rear panel The deuterium lamp emits UV radiation that is harmful to the eyes Always turn off the detector power before removing the lamp cover La lampe deuterium emettet de rayons ultraviolets qui sont dangeroux pour les yeux Voulez vous etteindre le detecteur avant d enlever le couvercle de la lampe AVERTISSEMENT gt Die Deuteriumlampe gibt UV Strahlung ab diese ist schadlich f r die Augen Schalten Sie den Detektor immer aus ehe Sie die Abdeckung von der Lampe entfernen WARNUNG gt The lamp housing and base may be hot to the touch especially after the lamp has been in operation for a long time Wait until the lamp has cooled down before continuing CAUTION gt La lampe et la base de la lampe peuvent tre chaudes au toucher particuli rement apr s que la lampe a t allum e pendant longtemps Attendez que la lampe ait refroidi avant de continuer MISE EN GARDE gt Das Lampengehause und die Lampenbefestigung konnen sehr hei werden besonders wenn die Lampe l ngere Zeit in Betrieb war Warten Sie bis die Lampe abgek hlt ist bevor Sie diese ber hren VORSICHT 4 5 6 Grasp the de
20. 4 14 Faulty USB Communication e Dionex PDA not recognized by Windows operating system Thermo Fisher Scientific strongly recommends installing Chromeleon before connecting the Dionex PDA to the computer When the chromatography software is installed first USB driver information is loaded automatically If Windows fails to detect the Dionex PDA refer to the following table for corrective action Problem Action Windows Vista fails to detect This indicates that you connected the Dionex PDA the Dionex PDA and to the computer and turned on the power for the launches a wizard instead first time before you installed Chromeleon To resolve the problem e Click Cancel to exit the wizard e Turn off the detector and unplug the USB cable from the computer Install Chromeleon e Reconnect the USB cable to the computer and turn on the power to the detector Windows Vista will now detect the Dionex PDA and automatically install the USB software for it Windows XP fails to detect This indicates that you connected the Dionex PDA the Dionex PDA and a to the computer and turned on the power for the message box asks fora USB first time before you installed Chromeleon To configuration file resolve the problem CmW dmUsb inf e Click Cancel in the Windows message box e Turn off the detector power and unplug the USB cable from the computer e Install Chromeleon e Reconnect the USB cable to the computer and turn on the power to
21. 5000 systems USB compatibility issues 121 Important icon 7 Inside front panel 13 Access to panel 13 Illustration 13 Installation Chromeleon 6 8 119 Doc 065378 01 1 12 Index 3 Dionex PDA Operator s Manual Chromeleon 7 119 Instructions 117 118 PDA with ICS 3000 system 121 PDA with ICS 5000 system 121 Site requirements 105 111 Instrument connections 74 Instrument method Chromeleon 7 41 Integrator Analog output connections 116 Input voltage 84 Isocratic applications Reference wavelength selection 48 79 L Lamp intensity 56 Lamp power supply board 21 Lamps 2 Calibration 80 DEUTERIUM UV LED is flashing 12 Failure 12 Installation procedures 98 101 See also Deuterium lamp See also Tungsten lamp TUNGSTEN VIS LED is flashing 12 Leak sensor 13 Leak tray 13 Maintenance 22 55 Leaks Prevention 22 Symptoms 55 LEDs on front of detector 12 Clearing the ALARM LED 73 Lenses 15 Liquid leaks 91 Liquid lines Maintenance 55 56 Lithium battery disposal 91 M Maintenance procedures 55 Mise en garde icon 8 Mobile phases 26 Concentration guidelines 16 25 43 Degassing 25 75 Effect of pH on retention time 25 Lamp stability after changing 75 78 Preparation 75 Reservoir material 26 Solvent quality 25 Temperature stabilization 17 18 Moduleware 21 Diagnostic procedures 59 87 N Negative absorbance 43 77 Definition 53 Guidelines for selec
22. Dionex PDA in Chromeleon The Chromeleon USB Auto Configuration Wizard appears automatically when a USB device that is not assigned to a Chromeleon 7 instrument or a Chromeleon 6 8 timebase is powered up You can use the wizard to create a new instrument or timebase for the Dionex PDA see Section B 10 1 If you prefer click Cancel to close the wizard and then manually create an instrument or timebase e For instructions on how to manually create an instrument refer to the Chromeleon 7 Help or Chromeleon 7 Installation Guide e For instructions on how to manually create a timebase refer to the Chromeleon 6 8 Help or to nstalling Chromeleon with a Dionex Ion Chromatograph Document No 031883 The software installation manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 B 10 1 Using the USB Auto Configuration Wizard 1 Review the names displayed under Unassigned USB Devices Detected Clear the check mark before the name of all devices other than the Dionex PDA 2 Under Mode select a predefined configuration template for the new instrument or timebase 3 Optional Select the Launch Instrument Controller Service upon closing this wizard check box Chromeleon 7 or the Launch Server Configuration upon closing this wizard check box Chromeleon 6 8 The check box is disabled if the program is already running Doc 065378 01 1 12 125 Dionex PDA Operator s Manual 4 Optional Select
23. If the sample wavelength is 272 nm you might select a reference wavelength of 325 nm because both wavelengths are within the UV spectrum 190 to 380 nm of the deuterium lamp Doc 065378 01 1 12 47 Dionex PDA Operator s Manual If the sample wavelength is 372 nm you might select a reference wavelength of 425 nm because both wavelengths are within the visible spectrum 380 to 800 nm of the tungsten lamp Select a reference wavelength and reference bandwidth in a quiet area of the spectrum where little absorption occurs The reference wavelength plus one half the reference bandwidth must be within the sample wavelength range selected if it is not the reference wavelength will default to the longest wavelength If the data collection rate is 20 Hz the 3D sample wavelength range must be lt 310 nm When programming a 3D channel the reference wavelength if set must be within the 3D range The reference wavelength plus one half the reference bandwidth must be within the sample wavelength range selected if it is not the reference wavelength will default to the longest wavelength The active reference mode minimizes baseline drift and is ideal for gradient analyses where the baseline may shift This mode also helps compensate for fluctuations in ambient temperature caused by air conditioning To cancel the active reference mode enter Off as the reference wavelength The intensity reading at the time of autozero will be used a
24. Inlet Tubing F 0 51 mm 0 020 in ID P N 042855 Handle ES EN Spring Clip Flow Cell Figure B 2 Semi Preparative Flow Cell Connections 9 Connect a length of 0 51 mm 0 020 in ID tubing P N 052308 to the cell outlet connection see Figure B 1 or Figure B 2 This is the cell waste line 114 Doc 065378 01 1 12 B Installation 10 Connect a backpressure line to the cell outlet The backpressure line will provide enough restriction to generate the small amount of backpressure 0 14 to 0 34 MPa 20 to 50 psi required to help prevent bubbles from forming in the cell a Locate the following items in the Dionex PDA Ship Kit P N 060977 0 25 mm 0 010 in ID tubing P N 052306 two split cone 10 32 ferrule fittings P N 062978 and two 10 32 bolts P N 064980 Cut the tubing to the required length 1 meter for a flow rate of 1 0 mL min 2 meters for a flow rate of 0 5 mL min and so on Install a 10 32 ferrule fitting and bolt on each end of the tubing Using a union fitting P N 042627 connect the backpressure line to the cell waste line installed in Step 9 The backpressure on the cell must not exceed 2 MPa 300 psi for a PEEK standard or semi micro cell 3 MPa 500 psi for a stainless steel standard or semi micro cell or 10 34 MPa 1500 psi for a semi preparative cell 11 Thread the cell outlet tubing through the slot near the bottom of the front cover Thread the cell inlet tubing thr
25. O ring from sealing IMPORTANT gt A properly and will cause leaks scratches in the groove particles of dust or dirt in the groove and failure to seat the new O ring in the groove Doc 065378 01 1 12 95 Dionex PDA Operator s Manual Cu Cell Outlet Tubing 4 Cell Inlet Tubing O Ring Groove WM O Ring P N 054136 Window P N 054135 Flow Cell Retaining Nut P N 054133 10 Figure 5 2 Replacing the Standard or Semi Micro Flow Cell Windows Light inlet side shown Check the groove to be sure it does not contain any dust or dirt particles and then install a new O ring P N 054136 Make sure the O ring is seated in the groove Place a new window P N 054135 into the counterbore in the retaining nut Screw the window into place Using the windows replacement tool tighten the retaining nut until snug and then turn an additional one quarter turn Repeat Step 3 through Step 8 to install the second window Connect the flow cell to the pump and pressurize to 1 38 MPa 200 psi Check for leaks around the windows If there is any leakage tighten the retaining nut s with the windows replacement tool just until the leak stops IMPORTANT Do not overtighten the retaining nut as this may fracture the window 96 Doc 065378 01 1 12 5 Service 11 If tightening the retaining nut s stops the leakage dry the cell thoroughly with a lint free optica
26. TUNGSTEN VIS POWER Figure 2 2 Dionex PDA Status Bar LED Label LED Status Function CONNECTED Lighted The Dionex PDA is connected to a Chromeleon 7 instrument or a Chromeleon 6 8 timebase Off The Dionex PDA is not connected to a Chromeleon 7 instrument or a Chromeleon 6 8 timebase ALARM Lighted A problem has occurred a leak for example Check the Chromeleon Audit Trail for the cause Off No problems have been detected DEUTERIUM UV Lighted The deuterium lamp is on Flashing The LED flashes once every second while the deuterium lamp is firing The LED flashes every 0 5 second if a command is issued to turn on the lamp but the lamp fails to turn on see Section 4 3 If a subsequent attempt to turn on the lamp is successful the LED will automatically stop flashing Off The deuterium lamp is off TUNGSTEN VIS Lighted The tungsten lamp is on Flashing The LED flashes once every second while the tungsten lamp is firing The LED flashes every 0 5 second if a command was issued to turn on the lamp but the lamp failed to turn on see Section 4 3 If a subsequent attempt to turn on the lamp is successful the LED will automatically stop flashing Off The tungsten lamp is off POWER Lighted The Dionex PDA power is on Off The Dionex PDA power is off 12 Doc 065378 01 1 12 Ze Description 2 2 Inside Front Panel Grasp the Dionex PDA front cover by
27. The Dionex PDA is controlled by a PC configured with either the Chromeleon 7 Chromatography Data System or the Chromeleon 6 8 Chromatography Data System Both software products provide extensive instrument control data management reporting and compliance features In Chromeleon 7 an ePanel Set provides centralized system control You can use the ePanel Set to view system status information and issue commands for controlling each module In Chromeleon 6 8 these functions are available on a panel tabset In both the ePanel Set and the panel tabset a convenient Home panel shows the overall system status and provides basic module control Doc 065378 01 1 12 27 Dionex PDA Operator s Manual functions The UV_Vis tab provides access to Dionex PDA functions as well as detailed status and diagnostics information Figure 2 9 shows the Dionex PDA ePanel in Chromeleon 7 o x Help 7 i p lt Autogenerated gt E Monitor Baseline 22 Command CQ Detach ePanel Smart Startup 8 Smart Shutdown Default Pump UV Vis Audit Startup Queue Device ICS 3000 PDA 30007 2000 Uv VIS 2 F Q connected Se UV_MIS_3 Base 2 UV_VIS_4 trok ontrols eos UV MG Lean E Pump 1 Pressure e e 4004 Pump_2_Pressure s UVLamp Vis Lamp UV_VIS_1 Data Collection 10 00 5 200 ECH 2 00 3 Rise Time E E La A Step Ave 7200 200 RAA 210 nm l
28. an inappropriate step setting may cause loss of sensitivity skipped data points and other problems Doc 065378 01 1 12 67 Dionex PDA Operator s Manual Leak sensor error To troubleshoot Locate the source of the leak and tighten or replace the liquid line connection For tightening requirements refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Thermo Scientific Reference Library DVD P N 053891 If the cell is leaking check that the backpressure on the cell does not exceed the specification see Section A 5 Wipe up all liquid and dry the leak sensor before resuming operation If the cell leaks after you resume operation replace it see Section 5 6 Not enough light to perform operation To troubleshoot Follow the troubleshooting steps in Section 4 7 Overtemperature error To troubleshoot The fan that cools the optical bench may have malfunctioned or a component on the lamp supply board may have failed Turn off the Dionex PDA power and contact Thermo Fisher Scientific for assistance NOTE Do not attempt to service the Dionex PDA electronics components All repairs of the electronics components must be performed by Thermo Fisher Scientific personnel 68 Doc 065378 01 1 12 4 Troubleshooting PDA is running a calibration or diagnostic function Not ready to accept this command To troubleshoot Wait until the c
29. fail are logged in the Audit Trail The result of the last wavelength verification test is stored in the calibration log and can be retrieved at any time NOTE Wavelength verification can take up to 2 minutes During this time data acquisition is not possible In Chromeleon 7 a Openthe Command window see page 39 click UV and execute the WavelengthVerTest command 88 Doc 065378 01 1 12 4 Troubleshooting In Chromeleon 6 8 a open the Wellness panel click the Wellness button on the Dionex PDA Control panel b Click the wavelength verification script button under Diagnostics Doc 065378 01 1 12 89 Dionex PDA Operator s Manual 90 Doc 065378 01 1 12 5 Service This chapter describes routine service procedures for the Thermo Scientific Dionex ICS Series Photodiode Array Detector Dionex PDA that users may perform All procedures not described here including electronics related repair procedures must be performed by Thermo Fisher Scientific personnel For assistance contact Technical Support for Dionex products In the U S and Canada call 1 800 346 6390 Outside the U S and Canada call the nearest Thermo Fisher Scientific office A The Data Processing board contains a lithium battery If the board is A di replaced dispose of the used battery according to local regulations Peng Before replacing any parts review the troubleshooting information in Chapter 4 to
30. flange of the new lamp with the two locating pins and three threaded holes in the optical bench see Figure 5 3 When the flange is aligned gently push the lamp into the optical bench 13 When the lamp is fully seated tighten the screws in the flange with a screwdriver IMPORTANT To ensure proper performance the lamp must be fully seated 14 Squeeze the clip on the UV lamp connector and insert it into the 6 pin bulkhead connector on the side wall Route the wires through the wire guide in the optical bench see Figure 5 3 Doc 065378 01 1 12 99 Dionex PDA Operator s Manual 15 Replace the lamp cover IMPORTANT Do not pinch the UV lamp connector wires under the lamp cover 16 17 Thread the flow cell inlet tubing through the tubing guide on the lamp cover and reinstall the tubing bracket Replace the flow cell cover and reconnect the inlet and outlet tubing IMPORTANT Do not pinch the tubing under the flow cell cover 18 19 20 2 22 Replace the detector front cover Turn on the detector power Start the Chromeleon instrument controller or server Reset the lamp lifetime a Openthe Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 b Select UV and then select the UVLampAge command c Resetthe lamp age to zero d Execute the command NOTE It is normal for the baseline to drift for several hours after a new deuterium lamp is instal
31. hours turn off the lamp for at least 30 seconds and then turn it on again If the error message reappears replace the lamp see Section 5 8 If the error message does not appear again run a manual data acquisition for about 30 minutes If you notice a shift in the absorbance signal during this time replace the lamp Doc 065378 01 1 12 71 Dionex PDA Operator s Manual UV lamp control circuitry error while lamp is off UV lamp error while attempting to turn off Visible lamp control circuitry error while lamp is off Visible lamp error while attempting to turn off To troubleshoot The lamp power supply may have failed or the CPU board may have failed Contact Thermo Fisher Scientific for assistance NOTE The Dionex PDA electronics cannot be serviced by users All repairs of the electronics components must be performed by Thermo Fisher Scientific personnel When collecting at 20 Hz the spectrum range cannot be more than 310 nm Please lower the data rate or narrow the spectrum range To troubleshoot Reduce the data collection rate to less than 20 Hz or select a wavelength range that is lt 310 nm 72 Doc 065378 01 1 12 4 Troubleshooting 4 2 4 3 ALARM LED Is Lighted The leak sensor in the drip tray may have been triggered Check the Chromeleon Audit Trail for a leak related error message Find and eliminate the source of the leak After fixing the leak and drying the sensor c
32. is installed 4 Plug the connector of the USB cable into a port on the external USB hub see Figure B 7 USB USB Device Device B B Plug the USB cable s A connector USB Cables into the USB port on the PC Plug the USB cable s B connector into the B port on the USB hub Figure B 7 Example USB Connections Modules Connected to an External Hub 122 Doc 065378 01 1 12 B Installation B 8 Connecting the Power Cord 1 Verify that the main power switch on the rear panel of the Dionex PDA is turned off The main power switch may be turned on accidentally when the detector is unpacked 2 Connect a modular power cord IEC 320 C13 from the Dionex PDA main power receptacle see Figure B 3 to a grounded single phase power source The power supply is auto sensing No adjustment is needed to select the line voltage SHOCK HAZARD To avoid elecirical shock use a grounded receptacle Do not operate the Dionex PDA or connect it to AC power without an earthed ground connection gt WARNING The power supply cord is used as the main disconnect device Make sure the socket outlet is located near the Dionex PDA and is easily accessible gt CAUTION Operation at AC input levels outside of the specified operating voltage range may damage the Dionex PDA gt CAUTION DANGER D ELECTROCUTION Pour viter toute lectrocution il faut utiliser une prise de courant avec prise de
33. misidentified as the same component HE 2 Calibration 4 modified by bclemons UV VIS 1 Calibration 5 Solvent Injection VIS 3 375 3 500 3 625 3 750 3 957 Figure 1 2 Overlay of Pyrene and an Impurity The Dionex PDA under the control of Chromeleon 6 8 with the 3D Data Acquisition license correctly identified and differentiated the components The spectra of pyrene and the impurity see Figure 1 3 clearly indicate that the two peaks are different components Doc 065378 01 1 12 1 Introduction Calibration 4 Compound 20 0 pl Pyren 3 51 60 0 Pyren 3 52 Impurity 40 0 20 0 10 0 200 250 300 350 400 450 500 595 Figure 1 3 Spectra of Pyrene and an Impurity Doc 065378 01 1 12 5 Dionex PDA Operator s Manual 1 3 Operator s Manual Overview The electronic version 1 e the PDF file of this manual contains numerous hypertext links that can quickly take you to other locations within the file These links include e Table of contents entries Index entries e Cross references underlined in blue to sections figures tables etc If you are not familiar with how to navigate PDF files refer to the Help system for Adobe Acrobat or Adobe Reader for assistance Chapter 1 An introduction to the Dionex PDA and the theory of Introduction photodiode array detection includes an explanation of conventions used in this manual Chapter 2 overv
34. not use a PEEK flow cell with normal phase or chlorinated solvents these solvents will damage the cell Do not use a stainless steel flow cell with low pH solutions these solutions may cause corrosion contamination and metal leaching Prepare all mobile phases with spectroscopy grade solvents reagent grade chemicals and ASTM Type I 18 megohm cm filtered deionized water that meets the specifications listed in Table B 1 Degas all mobile phases before use and maintain them in a degassed state Mobile phase pH affects not only the retention time of the separation but the sample absorbance and the background absorbance of the mobile phase If an analysis employs chemical suppression and compound detection techniques compare the UV cutoff of the mobile phase before and after the suppressor to see whether it is advantageous to locate the Dionex PDA ahead of the suppressor This location also limits suppressor exposure to backpressure When changing from a buffer to a different operating mobile phase be sure the solvents are miscible and will not induce precipitation of the buffers Flush the cell with deionized water immediately after the analysis Doc 065378 01 1 12 25 Dionex PDA Operator s Manual 2 6 2 Solvent Delivery System The pumping system should deliver continuous flow while maintaining a consistent mobile phase composition if gradient elution is used Fluctuations in system backpressure may cause basel
35. s manual To avoid contamination always wear latex gloves that are lint free particle free and oil free when handling pump components in the flow path Contamination may cause baseline disruptions spurious peaks and inconsistent results especially in sensitive applications 26 Doc 065378 01 1 12 2 Description To clean the pump and system between applications 1 Remove the column and the suppressor if installed 2 Connect the line exiting the injection valve directly to the flow cell inlet tubing 3 Flush the system with deionized water at 1 0 mL min for 20 minutes 4 Flush the system with methanol at 1 0 mL min for 20 minutes For very sensitive applications continue flushing for several hours 5 Flush the system with deionized water at 1 0 mL min for 15 to 20 minutes 6 Reinstall the column and the suppressor if removed and equilibrate the system before resuming operation If there is a heavy salt build up on the pump pistons remove the pistons and clean them with deionized water Refer to the pump user s manual for instructions Cleaning the pistons removes salt crystals that can abrade the piston thereby causing the main seal to wear out prematurely and allow leaks Replace the piston seals if there is a heavy salt build up on the pistons if the seals leak or if the pistons are replaced Refer to the pump user s manual for instructions 2 7 Chromatography Software 2 7 1 Overview
36. the Customize instrument names For advanced users only check box Chromeleon 7 or the Customize timebase names For advanced users only check box Chromeleon 6 8 Click Accept to create a new instrument or timebase If you selected the Customize instrument or Customize timebase option the Change Instrument Names or Change Timebase Names dialog box appears now Enter a new and unique name and click the Use Custom Names button To cancel click the Use Default Names button NOTE Selecting an instrument or timebase name already in use on another instrument controller or server can cause unpredictable behavior If you selected the Launch Instrument Controller Service or Launch Server Configuration option the program automatically starts running when you close the wizard If the Instrument Controller Service or Server Configuration was already running it is updated with the new configuration information 126 Doc 065378 01 1 12 B Installation B 10 2 Selecting Configuration Properties When the Dionex PDA is added to an instrument or timebase default configuration properties are selected Verify the default settings for the detector and select other settings as required 1 To open the configuration properties dialog box right click the detector in the instrument or timebase and click Properties The Properties dialog box for the detector appears see Figure B 8 Dionex PDA Photodiode Array D
37. the detector Windows will now automatically detect the Dionex PDA and launch the Found New Hardware Wizard 86 Doc 065378 01 1 12 4 Troubleshooting 4 14 1 4 14 2 Moduleware Run Time Diagnostics The Dionex PDA Moduleware periodically checks the status of certain system parameters All problems are reported to the computer and logged in the Chromeleon Audit Trail The Audit Trail includes the date time and severity level for each problem the Dionex PDA reports There are two ways to review this information Check the Audit Trail displayed on the Dionex PDA ePanel or Control panel Or e Retrieve the Audit Trail from a sequence by selecting the Audit Trail folder in the timebase and the file for that date Software Diagnostics and Calibration Chromeleon includes comprehensive diagnostics for the Dionex PDA This section describes some of the most frequently used diagnostic procedures For more information refer to the Chromeleon Help Lamp age Purpose Indicates the total number of hours that each lamp has been turned on in its lifetime To reset the lamp age a After installing a new lamp open the Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 b Select UV and then select the UVLampAge command for the deuterium lamp or VisLampA ge command for the tungsten lamp c Reset the number to zero d Execute the command NOTE When the detecto
38. the maximum absorbance wavelength for each peak can be determined A photodiode array detector can collect spectra of each peak after which the detector software can calculate the absorbance maximum Detection of multiple wavelengths A photodiode array detector can monitor a sample at more than one wavelength This is especially useful when the wavelength maxima of the analytes are different Wavelengths can be selected to analyze each compound at its highest sensitivity Peak purity analysis It is difficult to determine component purity from a chromatogram However a photodiode array detector can analyze peak purity by comparing spectra within a peak The better the spectra match the higher the possibility that the peak is pure Positive peak identification In liquid chromatography peak identification is usually based on relative retention times When a photodiode array detector is used Doc 065378 01 1 12 Dionex PDA Operator s Manual spectra are automatically collected as each peak elutes The detector software compares the spectra with those stored in a library to determine the best fit matches this method increases the likelihood of correctly identifying peaks For example Figure 1 2 shows an overlay of pyrene and an impurity obtained from two consecutive chromatographic analyses Based on 2D data or if the analyses had been performed with a conventional variable wavelength detector the peaks might have been
39. the sides and pull it straight off to access the inside front panel see Figure 2 3 Flow Cell Cover Power Button Figure 2 3 Dionex PDA Inside Front Panel e The flow cell cover protects the cell from dust ambient light fluctuations in ambient temperature and vibration e The lamp cover enhances the thermal stabilization of the optical bench The optical bench is housed in a compartment behind the inside front panel e Because the flow cell is located behind a cover leaks from the cell tubing connections will not be apparent immediately To prevent damage to detector components the bottom of the optical bench contains a built in leak tray A sensor in the sump of the leak tray responds to changes in the index of refraction when wet When the leak sensor is activated it triggers an alarm in the detector the ALARM LED lights see Figure 2 1 and an error message is logged in the Chromeleon Audit Trail After fixing the leak and drying the sensor clear the ALARM LED see Section 4 2 Doc 065378 01 1 12 13 Dionex PDA Operator s Manual 2 3 Optical System Figure 2 4 is a schematic of the Dionex PDA optical system Light from the tungsten lamp is focused through an opening in the internal structure of the deuterium lamp Light from the tungsten and deuterium lamps is then focused through the flow cell by the source lens After exiting the cell the light passes through the spectrograph lens to the
40. these symptoms Decreasing pressure this may indicate a leak A sudden increase in backpressure this may indicate plugged tubing A gradual increase in backpressure is normal as the separator column ages To troubleshoot bypass the column and then start the pump the backpressure should decrease substantially Doc 065378 01 1 12 55 Dionex PDA Operator s Manual Without the column backpressure is usually less than 0 34 MPa 50 psi depending on the flow rate and tubing ID Note that the semi micro flow cell will develop approximately 1 03 MPa 150 psi backpressure at 1 0 mL min If the backpressure remains high remove the fittings and tubing from part of the flow path section by section starting at the waste line work back upstream until you identify the section causing the substantial backpressure Replace tubing and fittings as necessary Periodically check the flow cell tubing connections for leaks or restrictions Replace tubing and fittings as necessary Periodically repassivate stainless steel systems This is especially important when operating with extreme pH levels which will shorten the life of the passivation finish or after a major disassembly For instructions see Passivation of Stainless Steel Systems and Components Document No 031152 Monitor baseline noise If the noise increases above an acceptable level especially after a lamp s has been in service for an extended length of time r
41. 05 Power supply 20 Preamp board 21 Preamp gain 21 Predictive Performance 30 Problems See Troubleshooting Processing method 41 Program Chromeleon 6 8 29 41 Properties dialog box 39 Pumping system requirements 26 Q Quantification method 41 R Rear panel Analog output connectors 22 Clearance required 78 Drain tube 22 Fuses 24 Illustration 22 116 Power cord connection 23 Relay TTL connectors 23 USB connector 23 Recorder Analog output connections 116 Input voltage 84 Reference bandwidth 43 Definition 50 Guidelines for selecting 46 48 50 Reference intensity 47 Reference modes 47 Active reference 47 48 78 See also Reference wavelength Turning off active reference 48 Doc 065378 01 1 12 Index 5 Dionex PDA Operator s Manual Reference wavelength 43 47 48 50 78 Definition 47 Effect on baseline drift 48 Guidelines for selecting 47 48 50 Inappropriate setting 76 Relay control 23 117 Installation 117 Pin assignments 118 Relay TTL connector 23 117 118 Part number 131 Replacing parts 91 Use of non Dionex parts 91 Retention time 25 Rise time 43 Correlation with data collection rate 45 Definition 44 Effect on baseline noise 44 Guidelines for selecting 44 45 Inappropriate setting 77 S Safety icons in this manual 7 8 Sample bandwidth Guidelines for selecting 46 Sample intensity 47 Sample rate See Data collection rate Sampl
42. 1 Resetting the lamp age 87 See also Lamps Time to stabilize 33 37 75 78 Twisted wire assembly 117 Part number 131 U USB 106 Communication problem 86 Connector on rear panel 23 Driver 118 USB cable Installation 120 122 USB compatibility issues With ICS 3000 systems 121 With ICS 5000 systems 121 UV commands In Chromeleon 6 8 40 In Chromeleon 7 40 UV wavelengths 15 Doc 065378 01 1 12 Index 7 Dionex PDA Operator s Manual V Verification wavelength 88 Visible focus lens 15 Visible wavelengths 15 Vorsicht icon 8 W Warning icon 7 Warnung icon 8 Warranty voiding 91 Waste line 22 Installation 116 Wavelength calibration 2 82 88 Causes of failure 82 95 Wavelength verification 15 82 88 Wavelengths single 1 46 Reference modes 47 Windows cell 15 Contamination 82 95 Cracked 97 Etching with strong bases 16 25 43 Replacement kit 95 Replacement procedure 95 96 Index 8 Doc 065378 01 1 12
43. 12 1 Dionex PDA Operator s Manual 1 2 Key features of the Dionex PDA include e The deuterium and tungsten lamps ensure low baseline noise high signal intensity and applications flexibility in the wavelength range from 190 to 800 nm e The 1024 element photodiode array optimizes spectral resolution e The built in holmium oxide filter verifies wavelength calibration accuracy e Five flow cells are available for standard semi micro and semi preparative applications e LEDs on the front cover provide detector status at a glance e Four analog outputs support data collection on alternate data collection systems e detector is controlled with a PC personal computer running Microsoft Windows Vista or Windows XP and either the Chromeleon 7 Chromatography Data System or the Chromeleon 6 8 Chromatography Data System Chromeleon 7 and Chromeleon 6 8 also provide data acquisition and data processing functions NOTE Thermo Scientific Dionex Chromeleon Xpress software can provide real time control and monitoring of the detector but does not include data management capabilities Theory of Photodiode Array Detection Monochromatic variable wavelength detectors monitor eluting components of the sample at a single wavelength ideally the wavelength of maximum absorbance Photodiode array detectors scan a range of wavelengths every few milliseconds and continually generate spectral information Wavelength time and
44. 6 1 2200 mAU 50 mAU 300 mAU 2300 mAU 100 mAU 350 mAU 2600 mAU 200 mAU 450 mAU 2600 mAU 300 mAU 550 mAU 2700 mAU 400 mAU 630 mAU 2700 mAU 500 mAU 660 mAU 2700 mAU 600 mAU 760 mAU These signals are saturated and will not report a further negative value Open the Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 and select UV Select NegativeAbsorptionLevel enter a new setting and execute the command Select Autozero and execute the command to run the autozero routine Select the LampIntensity command to check the intensity of the deuterium lamp The reading should be above 10 million counts for a standard or semi preparative cell or above 3 million counts for a semi micro cell If the reading is lower than it should be select UN Calibration Intensity and execute the command to calibrate the intensity of the deuterium lamp Afterward check the lamp intensity again If the reading is still too low clean the flow cell see Section 5 2 or replace the lamp see Section 5 7 You may continue increasing the negative absorbance level if the range is required however be aware that baseline noise may increase as the negative absorbance increases 54 Doc 065378 01 1 12 3 e Operation and Maintenance 3 5 Shutdown Before shutting down the Dionex PDA for more than 24 hours flush the system with deionize
45. 7 or Section 5 8 for instructions on replacing the deuterium lamp or tungsten lamp respectively Solvent absorbs at the wavelength reported for verification Pump deionized water or methanol through the system during the wavelength verification test Filter paddle position error Check the Chromeleon Audit Trail If the Filter wheel sensor could not detect blocked position or Filter wheel sensor could not detect open position message is displayed see page 66 for instructions 82 Doc 065378 01 1 12 4 Troubleshooting 4 10 No Spectra Collected Spectral range was not programmed In Chromeleon 7 select a spectral range in the instrument method or on the Dionex PDA ePanel In Chromeleon 6 8 select a spectral range in the program or on the Dionex PDA Control panel Detector and instrument method program or ePanel Control panel connected to different timebases In Chromeleon 7 add the detector to the same instrument as the instrument method or the Dionex PDA ePanel In Chromeleon 6 8 add the detector to the same timebase as the program or the Dionex PDA Control panel 4 11 Low Spectral Resolution Bunch width too wide Select a bunch width setting of 1 nm and then check the resolution again Bandwidth too wide Select a bandwidth that includes only the absorbing wavelength Incorrect reference wavelength Select a reference wavelength where minimum absorbance occurs Make sure the reference
46. Chromeleon Help 3 3 4 Direct Control With direct control you select operating commands and parameters from the following locations e Chromeleon 7 ePanel Sets or the Command window or e Chromeleon 6 8 Control panels or the Commands dialog box Direct control commands are executed as soon as they are entered Most routine direct control functions can be performed from ePanels or from Control panels For other functions you can use the Command window or Commands dialog box These provide access to all of the available commands and properties for the Dionex PDA as well as commands for other devices in the instrument or timebase respectively To issue direct control commands to the Dionex PDA 1 Open the ePanel Set see Section 3 1 2 or panel tabset see Section 3 1 3 and click the tab for the detector 2 Usethe controls buttons sliders etc on the panel to issue commands 38 Doc 065378 01 1 12 3 Operation and Maintenance 3 If the function that you want to perform is not available from the panel open the Command window see the instructions below or the Commands dialog box see page 40 The commands available in the Command window or Commands dialog box vary depending on these variables e The version of Chromeleon installed e The display filter level Normal Advanced or Expert e The options selected for the detector in the Properties dialog box in the Chromeleon 7 Instrument Config
47. Dionex ICS Series Photodiode Array Detector Operator s Manual Document No 065378 Revision 01 January 2012 2012 Thermo Fisher Scientific Inc All rights reserved BioLC and Chromeleon are registered trademarks of Thermo Fisher Scientific Inc in the United States Adobe Adobe Reader and Acrobat are registered trademarks of Adobe Systems Incorporated in the United States and other countries Microsoft Windows and Windows Vista are registered trademarks of Microsoft Corporation in the United States and other countries Tefzel is a registered trademark of E I duPont de Nemours amp Company in the United States and possibly other countries All other trademarks are the property of Thermo Fisher Scientific and its subsidiaries Thermo Fisher Scientific Inc provides this document to its customers with a product purchase to use in the product operation This document is copyright protected and any reproduction of the whole or any part of this document is strictly prohibited except with the written authorization of Thermo Fisher Scientific Inc The contents of this document are subject to change without notice All technical information in this document is for reference purposes only System configurations and specifications in this document supersede all previous information received by the purchaser Thermo Fisher Scientific Inc makes no representations that this document is complete accurate or error free and assumes no respon
48. Document No 031883 B 7 2 Chromeleon 7 Starting the Instrument Controller Service To start the Instrument Controller Service right click the Chromeleon tray icon which is crossed out in red and click Start Chromeleon Instrument Controller The icon changes to gold to indicate that the Instrument Controller Service is starting When the Instrument Controller Service is running idle the icon changes to gray KE If the Chromeleon tray icon is not on the taskbar click Start gt All Programs gt Chromeleon 7 gt Services Manager to open the Services Manager and click Start Instrument Controller B 7 3 Chromeleon 6 8 Starting the Server To start the Chromeleon server right click the Chromeleon Server Monitor tray icon which is crossed out in red Ge and click Start Server The icon changes to gold SS indicate that the Chromeleon server is starting When the server is running idle the icon is gray 88 If the Server Monitor icon is not on the taskbar click Start on the taskbar and select All Programs gt Chromeleon gt Server Monitor Click Start to start the server Doc 065378 01 1 12 119 Dionex PDA Operator s Manual B 7 4 Connecting the USB Cable Select one of the following methods to connect the Dionex PDA to the Chromeleon computer e Connect the detector directly to a USB port on the PC Connect the detector to the internal USB hub of another module in the system and connect the o
49. EI 40074 400 uv2 2541 S d 6004 7600 272nm S T Si uve S 9 pe min Uv5 600 g 2000 T T 14 1000 0 0 25 D 7 5 10 Dae Time Retention Device Message Figure 2 9 Example Dionex PDA ePanel in Chromeleon 7 28 Doc 065378 01 1 12 2 Description Figure 2 10 shows the Dionex PDA Control panel in Chromeleon 6 8 Figure 2 10 Example Panel Tabset in Chromeleon 6 8 Two modes of software control are available direct control and automated control With direct control you select operating parameters and commands from the Chromeleon 7 ePanels or Command window or the Chromeleon 6 8 Control panels or Commands dialog box Direct control commands are executed as soon as they are entered See Section 3 3 for details about direct control With automated control you create a Chromeleon 7 instrument method or a Chromeleon 6 8 program An instrument method or program is a list of control commands executed in chronological order for automated operation of the detector It can be created automatically with the help of a software wizard or manually by editing an existing instrument method or program See Section 3 3 for details about automated control Doc 065378 01 1 12 29 Dionex PDA Operator s Manual 2 7 2 2 7 3 3D Data Acquisition License To take full advantage of the Dionex PDA s capabilities order Chromeleon with the 3D D
50. Manual 2 7 Chromatography Software 27 271 Cheese e A 27 2 7 2 Data Acquisition License esee 30 2 7 3 System Wellness and Predictive Performance 30 3 Operation and Maintenance 33 Al Getting Started EE 33 3l Initial Startup sisse ee RR AD e 33 3 1 2 Connect to the Chromeleon 7 Client 34 3 1 3 Connect to the Chromeleon 6 8 Client 35 3 1 4 Turn On the Lamps 37 3 2 System Equilibration 37 3 3 Routine 38 3 31 Direct Control EELER EE E 38 3 3 2 Automated Control 41 3 3 3 Stand Alone Analog Operation 41 3 4 Optimizing Detector Performance 43 3 5 Shutdown yida EEN EISE EEN e NEEN SEN EN yr 55 3 6 Routine Maintenance 55 4 Troubleshooting 59 4 1 Alarms and Error Conditions 59 42 ALARM LED Is Lighted 73 4 3 Lamp Does Not Light Lamp LED Is Flashing Rapidly 73 Doc 065378 01 1 12 Contents 4 4 Detector Response 74 AS Noisy Baseline 4i des and ques eee dores 75 4 6 Drifting Ba
51. Photodiode Array Wavelength Range Pixel Resolution Wavelength Accuracy Noise with Standard or Semi Preparative Cell Installed Noise with Semi Micro Cell Installed Drift Linearity Analog Outputs Voltage Out Analog Output Range Control and Data Evaluation Single beam reverse optics design with concave holographic grating Deuterium lamp 30 W for ultraviolet spectrum analysis Tungsten lamp 15 W for visible spectrum analysis Both lamps Lifetime of 2000 hours with gt 50 of initial intensity 1024 element photodiode array bench 190 to 800 nm 0 7 nm 1 nm self calibration with deuterium lines verification with built in holmium oxide filter lt 10 LAU at 254 nm 2 second rise time 4 nm bandwidth and flowing water at 1 0 mL min lt 15 LAU at 520 nm 2 second rise time 10 nm bandwidth and flowing water at 1 0 mL min lt 15 LAU at 254 nm 2 second rise time 4 nm bandwidth and flowing water at 1 0 mL min lt 15 at 520 nm 2 second rise time 10 nm bandwidth and flowing water at 1 0 mL min 1000 n AU hour after warm up Deuterium lamp gt 2 AU Tungsten lamp gt 2 AU Four 0 to 3 AU selectable 1000 mV range V output 0 0005 0 001 0 01 0 1 0 5 1 0 2 0 or 3 0 AU full scale Provided by Chromeleon 7 or Chromeleon 6 8 software the PC and the detector are connected through USB Universal Serial Bus 106 Doc 065378 01 1 12 A Specifications
52. SB cable into the USB receptacle on the Dionex PDA rear panel Module with Internal USB Hub PDA C USB Cable Figure B 6 Example USB Connections Dionex PDA Connected to a Module with an Internal USB Hub Doc 065378 01 1 12 121 Dionex PDA Operator s Manual IMPORTANT Plug the USB cable s B connector into the USB receptacle on the PDA Plug the USB cable s A connector into the A port on the USB hub To connect the Dionex PDA to an external USB hub The Dionex PDA Ship Kit P N 060977 contains one USB cable P N 063246 Contact Thermo Fisher Scientific to order the external USB hub P N 060392 and additional USB cable P N 063246 required for this configuration The USB standard limits the USB cable length to 5 meters 5 5 yds Each USB device can be separated from the PC by no more than five hubs Thus if five hubs are installed each USB device can be located no more than 30 meters 32 yds from the PC Carefully secure all USB cables the USB hub and the hub power cable so that they cannot be accidentally disconnected 1 Plug the A connector of a USB cable P N 063246 into a port on the external USB hub P N 060392 see Figure B 7 2 Plug the connector of the cable into the USB receptacle on the Dionex PDA rear panel 3 Plug the A connector of the second USB cable P N 063246 into a USB port on the computer on which Chromeleon
53. This setting is recommended for most applications When Average is Off Chromeleon 6 8 reports the data points at the step interval The data points between steps are skipped and noise is not reduced If Average is On and the step size is more than double the rise time IMPORTANT A the system response is dominated by the step size The system response time is approximately the larger of a the rise time or b two times the step size when Average is On Negative Absorbance Negative absorbance is the result of decreased baseline absorption of the mobile phase after the autozero routine which usually occurs at the beginning of a run At the default setting of 1 the Dionex PDA becomes saturated when the light transmission 1s 2096 above the autozero level This results in a flat truncated baseline If desired increase the negative absorbance level in order to continue seeing the actual baseline and peaks This is especially helpful when running a gradient application in which the absorbance decreases more than 100 mAU As the following table indicates the extent of negative absorbance depends on the wavelength The values in this table are intended as guidelines only Doc 065378 01 1 12 53 Dionex PDA Operator s Manual Negative Approximate Negative Approximate Negative Approximate Negative Absorbance Absorbance 210 Absorbance 240 Absorbance at 254 nm Level 0 1 default 2 3 4 5
54. UV VIS 1 89 UV VIS 2 UV Vis 3 xg Uv VIS 4 UV VIS 5 v The System device contains commands and properties for the entire timebase lt is always available and can t be seen in Server Configuration Command Figure 3 4 Commands Dialog Box 3 o see the commands available for the Dionex PDA click the plus sign next to UV To execute a command click the Execute button NOTE change the display filter level right click the list of commands and select the desired filter on the context menu 40 Doc 065378 01 1 12 3 e Operation and Maintenance 3 3 2 Automated Control You can control the detector automatically by running instrument methods in Chromeleon 7 or programs in Chromeleon 6 8 that specify the function the detector and other system instruments should perform at a specific time Instrument methods and programs can be created automatically with the help of a software wizard or manually by editing an existing instrument method or program To prepare for automated control create a sequence a list of injections and specify the instrument method or program to run on each injection The sequence also includes a processing method in Chromeleon 7 or a quantification method in Chromeleon 6 8 for peak identification and area determination The table below lists the main steps required to set up and run the detector automatically Refer to the Chromeleon Help for details about these steps
55. absorbance can all be plotted Photodiode array detectors provide three dimensional information that allows an accurate assessment of peak identity purity and quantitation in a single analysis Software support for photodiode array detectors includes peak purity and spectral library search functions to help determine peak homogeneity and identity Doc 065378 01 1 12 1 Introduction 1 2 1 Advantages of Photodiode Array Detection Photodiode array detectors are useful in both research and quality assurance laboratories In the research laboratory the photodiode array detector provides the analyst with a variety of approaches to the analysis In the quality assurance laboratory the photodiode array detector provides several results from a single analysis thereby increasing the throughput of the HPLC Photodiode array detection offers the following advantages Peak measurement at all wavelengths In methods development detailed information about the detector conditions required for the analysis may not be known When a variable wavelength detector is used a sample must often be injected several times with varying wavelengths to ensure that all peaks are detected When a photodiode array detector is used a wavelength range can be programmed and all compounds that absorb within this range can be detected in a single analysis Determination of the correct wavelengths in one analysis After all peaks have been detected
56. aching the data processor Check that at least one lamp is turned on When a lamp is on the corresponding LED DEUTERIUM UV or TUNGSTEN VIS is lighted If necessary turn on one of the lamps from Chromeleon or the TTL input Low light throughput 1 Remove the cell from the optical bench see Section 5 4 2 Check the deuterium lamp intensity a Openthe Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 b Select UV and then select LamplIntensity If the lamp intensity reading is above 10 million counts for a standard or semi preparative cell or above 3 million counts for a semi micro cell follow these steps a Open the Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 b Select UV and then select UN Calibration Execute the Intensity command to calibrate the lamp intensity d Execute the Autozero command to run the autozero routine e If no error message is displayed flush the cell with the mobile phase for the application and or clean the cell as instructed in Section 5 2 Doc 065378 01 1 12 79 Dionex PDA Operator s Manual f Reinstall the cell in the optical bench g Autozero the detector again to verify that the problem has been resolved If the error message appears again contact Thermo Fisher Scientific for assistance If the lamp intensity reading is below 10 million counts for a standard or sem
57. alibration procedure or diagnostic routine finishes running before attempting to issue any command The minimum wavelength must be less than the maximum wavelength Min wavelength x max wavelength x To troubleshoot Select a minimum wavelength that is less than the maximum wavelength Both wavelengths must be within the 190 to 800 nm range The range of wavelength bunching is 1 to 25 nm To troubleshoot This message appears if you enter an invalid setting for the bunch width Select a bunch width setting from 1 to 25 nm The range of wavelengths is outside the 190 to 800 nm limit A Wavelength x Bandwidth x To troubleshoot The Dionex PDA can measure the absorbance spectrum from 190 to 800 nm Make sure both the minimum and maximum wavelengths are within this range Doc 065378 01 1 12 69 Dionex PDA Operator s Manual UV lamp error UV lamp error or control circuitry error while lamp is on UV lamp failed to turn on for the required operation UV lamp error while attempting to turn on Visible lamp error Visible lamp error or control circuitry error while lamp is on Visible lamp error while attempting to turn on Visible lamp failed to turn on for the required operation To troubleshoot 1 Check that the lamp referred to in the error message is turned on When a lamp is on the corresponding LED DEUTERIUM UV or TUNGSTEN VIS is lighted If necessary turn on the lamp fr
58. aligned with the two locating pins in the optical bench see Figure 5 3 If the flange is aligned the lamp is defective and should be replaced see Section 5 7 If the error message appears again contact Thermo Fisher Scientific for assistance Doc 065378 01 1 12 81 Dionex PDA Operator s Manual Flow cell contains air bubble or old mobile phase Flush the cell with the mobile phase for the application Cell not clear Clean the cell see Section 5 2 If the detector fails the wavelength calibration again replace the flow cell windows see Section 5 5 Contaminated flow cell windows can significantly increase baseline noise and cause wavelength calibration to fail 4 9 Wavelength Verification Fails Detector wavelength requires recalibration Open the Dionex PDA Wellness panel and run the wavelength calibration procedure see Section 4 14 2 No solvent flow through cell Check the Chromeleon Audit Trail If the Not enough light to perform operation message is displayed flush the cell with deionized water or methanol until the autozero routine can be performed without error Lamp s needs replacement Check the number of hours the lamps have been in service 1 Open the Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 2 Select UV and then select UVLampAge and VisLampAge If a lamp has been in service for more than 2000 hours replace it See Section 5
59. ata Acquisition license This license is required in order to perform 3D data presentation and spectral analysis real time or post run peak purity analysis with selectable criteria and spectral library search for positive peak identification Chromeleon supports a maximum of two detectors that can record a 3D field for example photodiode array or electrochemical detectors on one Chromeleon 7 instrument controller or Chromeleon 6 8 instrument server The total number of 3D data channels one instrument controller or server can acquire simultaneously depends on computer performance A 3D Data Acquisition license is not required to display and process data only to acquire it Thus data acquired on a station equipped with the 3D Data Acquisition license can be reviewed and processed on any Chromeleon client station System Wellness and Predictive Performance System Wellness monitors the overall health of the chromatographic system It provides built in diagnostic and calibration features that help prevent unscheduled system shutdowns and assure reliable operation of system devices Predictive Performance provides various functions for estimating the lifetime of replaceable parts and for planning and recording service and qualification procedures A partial list of the System Wellness and Predictive Performance features is provided below Refer to the Chromeleon Help for a complete list of the available features e Recording of d
60. avelength Output 1 210 10 Off 1 0 AU 10 2 254 10 Off 1 0 AU 10 3 272 10 Off 1 0 AU 10 4 520 10 Off 1 0 AU 10 These default settings are also in effect when the power is first turned on Rise time 2 0 seconds UV lamp On e Visible lamp On Stand Alone Operation The table below indicates which Dionex PDA parameter each TTL input controls during stand alone operation TTL Input Dionex PDA Parame ter TTL 1 in Autozero TTL 2 in Reserved TTL 3 in Deuterium lamp on off TTL 4 in Tungsten lamp on off 42 Doc 065378 01 1 12 3 Operation and Maintenance 3 4 Optimizing Detector Performance The performance of the Dionex PDA can be optimized by careful selection of key operating parameters This section defines these parameters describes how they interact and offers guidelines for selecting them The table below summarizes the topics discussed in this section Operating Parameter Flow cell material Rise time Data collection rate Sample wavelength Bandwidth Reference wavelength Reference bandwidth Bunch width Step Average Negative absorbance Performance Characteristics Affected Chemical compatibility Peak resolution sensitivity baseline noise Peak resolution disk space Sensitivity linearity Sensitivity vs baseline noise Baseline drift Baseline noise baseline drift Spectral resolution peak match disk space Baseline noise rise time data collection rate disk space Rise
61. baseline signal is at the expected reading for your application and is stable This may not be the case if the solvent composition has been modified or if the light path contains air bubbles See Section 4 5 and Section 4 6 for troubleshooting information NOTE To achieve optimum results allow 20 to 30 minutes for the lamp s to stabilize before beginning operation For sensitive applications work or for detector validation allow at least 2 hours for the lamps to stabilize Select one of the following methods to perform the equilibration tasks Select operating commands and parameters directly from the Chromeleon 7 ePanel Set or the Chromeleon 6 8 Control panel See Section 3 3 1 for details about direct control Doc 065378 01 1 12 37 Dionex PDA Operator s Manual 3 3 e Create and run an equilibration instrument method or program to automate the process See Section 3 3 2 for details about automated control e If you are running Chromeleon you can use the Smart Startup feature to automate system startup and equilibration In Chromeleon 7 you first create an instrument method from which the Smart Startup settings are derived In Chromeleon 6 8 you can use the Smart Startup Wizard to create a Smart Startup program Refer to the Chromeleon Help for details Routine Operation This section provides a brief overview of detector control with Chromeleon 7 or Chromeleon 6 8 For complete operating instructions refer to the
62. but the current run is not interrupted A Error A message is displayed in the Audit Trail and the system attempts to correct the problem sometimes by using an alternative parameter Abort A message is displayed in the Audit Trail and the running batch is aborted Doc 065378 01 1 12 59 Dionex PDA Operator s Manual The table below lists the Dionex PDA related error messages and their default severity levels For troubleshooting assistance refer to the page indicated in the table Dionex PDA Related Alarms and Error Conditions 3DFIELD RefWavelength and or RefBandwidth is out of range Acquisition On for 3DFIELD rejected no 3D Data Acquisition license found Autozero is already in progress Calibration is running Cannot change 3DFIELD parameters while data acquisition is running Cannot set manual parameters for the required operation because the DSP is not ready Can t execute calibration command during data acquisition Can t execute diagnostic command during data acquisition Can t execute x command during data acquisition Command not executed because an Autozero command is already running Data is unavailable Diagnostic is running DSP communication failure Filter wheel sensor could not detect blocked position Filter wheel sensor could not detect open position Invalid rise time Valid rise times at 20 Hz 0 05 0 1 0 2 0 5 1 0 and 2 0 Invalid step for the 3DFIELD Val
63. d leicht zuganglich ist gt VORSICHT Fuses The fuse holder is part of the main power receptacle The Dionex PDA uses two fast blow IEC 127 fuses P N 954763 rated at 4 0 amps For instructions on how to replace the fuses see Section 5 9 For continued protection against risk of fire or shock replacement fuses must be the type and rating specified here WARNING Pour maintenir la protection contre les risques d incendie ou d lectrocution remplacez toujours les fusibles par des fusibles du m me type et du m me calibre gt AVERTISSEMENT Zum Schutz vor Feuer und Stromschlagen m ssen beim Sicherungswechsel immer Sicherungen des gleichen Typs und mit gleicher Leistung verwendet werden WARNUNG 24 Doc 065378 01 1 12 Ze Description 2 6 Operating Guidelines 2 6 1 Mobile Phases Solvent quality significantly affects both detection limits and instrument performance To ensure optimal performance of the Dionex PDA observe the following precautions Strong bases can etch the fused silica windows of the flow cell If the mobile phase is a base make sure the mobile phase concentration does not exceed 0 1 M If the concentration of the base is greater than 50 mM disconnect the separator column and flush the system with deionized water for 5 minutes at 1 0 mL min immediately after the analysis If strong base remains in the cell for 1 to 2 days the cell windows may need to be replaced see Section 5 5 Do
64. d water or methanol for at least 15 minutes at 1 0 mL min or maintain a continuous flow at 0 2 mL min This rinses corrosive acids salts or bases from the flow paths The Smart Shutdown feature in Chromeleon 7 or Chromeleon 6 8 can assist you in creating and running a shutdown or standby procedure e shutdown process shuts down the system by automatically stopping the pump flow turning off the detector lamps and turning off heating in any temperature controlled devices that are installed e The standby process lets you quickly restart the chromatography system from standby A typical standby process includes steps such as reducing the pump flow rate and turning off heating in temperature controlled devices While the system is in standby mode the detector lamps remain on Both processes maintain the equilibrated status of an instrument until the system is restarted 3 6 Routine Maintenance The following maintenance procedures may be performed by users All other maintenance procedures for the Dionex PDA must be performed by Thermo Fisher Scientific personnel e Periodically check the drain tube connected to the leak tray at the bottom of the optical bench Verify that the tubing is unclogged and that it is routed below the leak tray e Periodically check all tubing and fittings and replace as necessary see Section 5 1 Tubing and fitting components may eventually become loose and leak or pinched off and plugged Look for
65. e analog recorder outputs Doc 065378 01 1 12 21 Dionex PDA Operator s Manual 2 5 Rear Panel Figure 2 8 illustrates the rear panel of the Dionex PDA Analog Outputs 4 Drain Tube Connector Relay TTL Connectors USB Connector Fuse Holder Power Entry 0606 6 Figure 2 8 Dionex PDA Rear Panel ANALOG OUTPUT Connectors The four analog outputs are standard female BNC connectors The output range is 0 to 1 volt The full scale absorbance range can be set to 0 0005 0 001 0 01 0 1 0 5 1 0 2 0 or 3 0 AU full scale in Chromeleon For details about programming the analog outputs see Section 3 3 2 The analog outputs will continue to output data after the PC is turned off or is disconnected from the Dionex PDA When the detector power is turned on again the analog output settings will be either the factory defaults see Section 3 3 3 or the settings selected the last time the detector was controlled by the computer Drain Tube Connector Waste exits the detector via a drain tube P N 055075 connected at the rear panel When correctly installed the drain tube is routed downward below the leak tray For installation instructions see Section B 4 IMPORTANT Check periodically to verify that the drain tube is not clogged or bowed upward and that the tubing remains routed below the leak tray If the drain tube is above the drain port the drip tray may back up and overflow inside the d
66. e wavelength Guidelines for selecting 46 Semi micro flow cells 15 Chemical compatibility 108 Flow rate range 16 Heat exchanger volume 16 Operating pressure 107 Optical path length 16 107 Overview 16 Replacement procedure 97 See also Cells Volume 16 107 Windows replacement 95 96 Windows replacement kit 95 Semi preparative flow cells 15 Chemical compatibility 108 Flow rate range 16 Heat exchanger volume 16 Operating pressure 108 Optical path length 16 108 Overview 16 Replacement procedure 97 See also Cells Volume 16 108 Windows replacement 95 Sensitivity 43 Separator column 55 Sequence 41 Server Configuration program Starting 35 119 Server Monitor 35 119 Service procedures Cell cleaning 93 Cell replacement 97 Cell window replacement 95 Deuterium lamp replacement 98 Eliminating liquid leaks 91 Fuse replacement 103 Removing air trapped in cell 93 Tungsten lamp replacement 101 Ship Kit PDA 112 122 Shutdown Smart Shutdown 55 Shutdown procedure 55 Signal intensity 47 Slit optical 14 15 Smart Shutdown 55 Solvents Chlorinated 17 25 43 113 Normal phase 17 25 43 113 Source lens 14 15 Spare parts 131 Spectra not collected 83 Spectral analysis 30 Spectral library 2 4 Spectral library search 30 Spectrograph lens 14 15 Spectrum 14 15 Improving resolution 83 Index 6 Doc 065378 01 1 12 Index Stainless steel flow cells 16 C
67. ep setting selected by Chromeleon 6 8 is the preferred setting However it is possible to override this setting by manually changing the step in the Chromeleon 6 8 program or on the Control panel For example you may want to increase the step time for the 3D field or any of the five absorbance channels For the 3D field the 52 Doc 065378 01 1 12 3 e Operation and Maintenance step determines the sampling rate at which the detector stores spectra Ideally the step is no smaller than the interval suggested for the rise time see the table in Data Collection Rate on page 45 The advantage of a larger step size is that it reduces the amount of data stored for example selecting a step twice as large as that listed in the table reduces the data file size for the 3D field by 50 If you select a larger step size when the average parameter is on see Average Chromeleon 6 8 only on page 53 the system response is a combination of the selected rise time and the average of the data points between steps If you select a larger step size when the average parameter is off the selected rise time is valid but some data points will be skipped Average Chromeleon 6 8 only The Average parameter operates in conjunction with the Step parameter see Step Chromeleon 6 8 only on page 52 When Average is On Chromeleon 6 8 averages the data points between step intervals reports that value and noise is reduced
68. eplace the lamp To check the lamp lifetime 1 Open the Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 2 Select UV and then select UVLampAge and VisLampAge If a lamp has been in service for more than 2000 hours replace it See Section 5 7 or Section 5 8 for instructions on replacing the deuterium lamp or tungsten lamp respectively Check the deuterium lamp intensity approximately every 6 months 1 Open the Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 2 Select UV and then select LampIntensity The reading should be above 10 million counts for a standard or semi preparative cell or above 3 million counts for a semi micro cell 3 Ifthe lamp intensity reading is too low calibrate the intensity In the Command window or Commands dialog box select UV_Calibration select Intensity and execute the command 56 Doc 065378 01 1 12 3 e Operation and Maintenance 4 After calibrating the lamp check the intensity again If the reading is still too low follow the steps in Section 4 7 to resolve the problem e Run the wavelength verification test for both the deuterium and tungsten lamps approximately every 6 months see Section 4 14 2 If a lamp fails the test calibrate the wavelength see Section 4 14 2 and then run the wavelength verification test again If a lamp fails the test again replace it For lamp rep
69. erence Bandwidth The reference bandwidth is analogous to the conventional bandwidth of a channel The purpose of the reference bandwidth is to average several photodiode signals in arange surrounding the reference wavelength It is not necessary to select a reference bandwidth unless you enter a reference wavelength i e you select the active reference mode If you enter Off as the reference wavelength the reference bandwidth will be the same as the bandwidth If you specify a reference bandwidth it should meet the following criteria Select a reference bandwidth in an area of the spectrum where the sample does not absorb Select a reference bandwidth that is narrow enough not to interfere with nearby compounds A wider bandwidth will reduce baseline noise but may increase the chance that the sample absorbs in the reference bandwidth this will reduce sensitivity The reference wavelength plus one half the reference bandwidth must be within the sample wavelength range selected The reference wavelength if set must be within the 3D range If the active reference mode is selected see Reference Wavelength on page 47 select a reference wavelength and reference bandwidth in a quiet area of the spectrum where little absorption occurs The reference wavelength plus one half the reference bandwidth must be within the sample wavelength range selected if it is not the reference wavelength will default to the longest wavelength If
70. erial number 46 9 34 10 AM TC TC 3000 Serial Demo Firmware Version 99 99 2 34 10 AM Column A Chip card detected 4 10 AM Column B Chip card detected reo 25 2 Chi Ka Kg Dn 2 Su EB 20m E 10 nm E ot 10 nm E Show Plot Show 34 Pio vis Lamp Figure B 10 Example Dionex PDA Control Panel in Chromeleon 6 8 Doc 065378 01 1 12 129 Dionex PDA Operator s Manual 130 Doc 065378 01 1 12 Part Number 939016T 056123T 954763 923686 043598 063246 056346 057304 055903 043276 043275 060498 056126 056124 055902 010262 010261 060498 064169 057304 055903 043276 043275 C Reordering Information Item Deuterium lamp Tungsten lamp Fuse 4 0 amps fast blow IEC 127 Relay TTL connector 12 pin Twisted wire assembly 2 meters 8 ft USB cable 1 m 3 ft Standard Flow Cell PEEK PEEK standard flow cell with heat exchangers PEEK standard flow cell outlet tubing assembly Reducing union fitting PEEK Ferrule Nut Dionex AD25 Dionex PDA Dionex PDA 100 Flow Cell Windows Replacement Kit Standard Flow Cell 316 Stainless Steel Stainless steel standard flow cell with heat exchangers Stainless steel standard flow cell outlet tubing assembly Reducing union fitting stainless steel Ferrule Nut Dionex AD25 Dionex PDA Dionex PDA 100 Flow Cell Windows Replacement Kit Semi Micro Flow Cell PEEK PEEK semi micro flow cell with heat exchangers PEEK semi
71. erver 20 Resetthe lamp lifetime a Openthe Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 b Select UV and then select the VisLampAge command c Resetthe lamp age to zero d Execute the command NOTE Before resuming routine operation allow 20 to 30 minutes for the lamp to stabilize 102 Doc 065378 01 1 12 5 Service 5 9 DANGER DANGER ACHTUNG NY placing the Main Power Fuses HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the Dionex PDA HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du Dionex PDA HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite des Dionex PDA Press the power button on the front of the Dionex PDA to turn off the power Turn off the main power switch on the Dionex PDA rear panel Disconnect the power cord from the Dionex PDA rear panel The fuse holder is part of the main power receptacle see Figure 5 4 Note the recessed lock on each side of the fuse holder Using a small screwdriver or your fingernails push one of the locks toward the center to release it The fuse holder will pop out slightly when the lock is released Repeat for the other lock Pull the fuse holder straight out of the compartment Fuse Holder Locki Fuses 2 Spina Locki
72. et 27 36 128 PDA Wellness panel 88 89 Peak purity analysis 30 Program 29 41 Properties dialog box 39 Quantification method 41 Running a program 41 Sequence 41 Spectral analysis 30 Spectral library search 30 Starting the client 35 System Wellness 30 USB driver information 118 Chromeleon 7 2 3D Data Acquisition license 30 Audit Trail 13 59 87 Automated control 41 Command window 39 Diagnostic procedures 87 Direct control 38 Direct control mode 38 ePanel Set 27 Installation 119 Instrument method 41 Overview of automated control 41 Peak purity analysis 30 Processing method 41 Properties dialog box 39 Running an instrument method 41 Sequence 41 Spectral analysis 30 Spectral library search 30 Starting the client 34 System Wellness 30 USB driver information 118 Chromeleon Server Starting 35 119 Chromeleon Xpress 2 Command window Opening 39 Selecting a display filter 40 Commands dialog box Opening 40 Selecting a display filter 40 Components elute slowly 75 CONNECTED LED LED is lighted 12 Control panel 36 129 D Danger icon 7 Dark signal 15 Data collection rate 43 Correlation with rise time 45 Definition 45 Guidelines for selecting 45 Relationship to step 52 Data files occupy too much disk space 45 Data points 45 52 Minimum number per peak 45 Data Processing board 21 117 Analog output connectors 21 Lithium battery disposal 91
73. etector 22 Doc 065378 01 1 12 Ze Description RELAY TTL Connectors TTL inputs control the following detector functions autozero TTL1 UV lamp on off TTL3 and visible lamp on off TTL4 The TTL2 input is reserved The two TTL outputs and two relay outputs can be programmed as part of a Chromeleon 7 instrument method or Chromeleon 6 8 program see Section 3 3 2 or controlled manually in the software The relay outputs can be programmed to switch any low voltage control The switched current must be less than 200 mA and 42 V peak The Dionex PDA Ship Kit P N 060977 includes a 12 pin connector P N 923686 for relay and TTL connections For installation instructions see Section B 6 USB Connector The USB connector allows communication between the Dionex PDA and the PC on which Chromeleon is installed The Dionex PDA Ship Kit P N 060977 includes one USB cable P N 063246 For installation instructions see Section B 7 4 Power Entry The Dionex PDA power entry is socketed for a modular power cord IEC 320 C13 The detector operates from input voltages over a range of 85 to 265 VAC 47 to 63 Hz power and requires a grounded single phase power source The typical input power is 100 W and the maximum line draw is 3 5 amps at 110 VAC when the detector power is turned on The appropriate line voltage and frequency are selected automatically NOTE Always leave the main power switch on unless instructed to tur
74. etector Demo Chromatogram Calibration Diagnostics General Signals State Devices EnorLevels Device Name UV Mode 2 Module Serial No 1 Use Live mode to control physical module connected to the server Virtual mode can be used to demonstrate the software support for the module and allows one to create methods and panels without having a physical module attached to the server Cancel Figure B 8 Dionex PDA Properties Dialog Box Review the default settings for the detector and change any settings that are not correct for your system If you have questions about parameters click the Help button When you finish click OK to close the dialog box On the File menu click Save Installation to save the configuration Doc 065378 01 1 12 127 Dionex PDA Operator s Manual B 11 Starting the Chromeleon Client Chromeleon 7 Client 1 2 Click Start gt All Programs gt Chromeleon 7 gt Chromeleon 7 To display the Chromeleon 7 ePanel Set click the Instruments Category Bar on the Console Chromeleon 7 connects to the instrument and displays the ePanel Set To view the Dionex PDA ePanel see Figure B 9 click the UV_Vis tab on the ePanel Set The ePanel provides access to Dionex PDA functions as well as detailed status and diagnostics information x 5 lt Autogenerated gt E Monitor Baseline 222 Command
75. etector check the Chromeleon Audit Trail If the Filter wheel sensor could not detect blocked position or Filter wheel sensor could not detect open position message is displayed see page 66 for instructions e Pump needs priming and or maintenance If the baseline noise is synchronized with the pump stroke reprime the pump and clean the piston seals and or check valves Refer to the pump user s manual for instructions Negative absorbance level is too high Baseline noise may increase as the negative absorbance increases If the noise is unacceptable reduce the negative absorbance level see page 53 Doc 065378 01 1 12 77 Dionex PDA Operator s Manual 4 6 Drifting Baseline Fluctuations in ambient temperature Make sure the Dionex PDA installation site temperature remains consistent Allow at least 6 cm 2 4 in of clearance behind the Dionex PDA for ventilation Check that the flow cell inlet tubing is routed through the heat exchanger see Figure 2 5 and is correctly connected to the inside front panel see Figure 5 2 Check that solvent flow is directed to the cell inlet and out the cell outlet Select the active reference mode by entering a reference wavelength see page 47 Front cover lamp cover or flow cell cover is missing Optical components are sensitive to temperature and light Do not operate the Dionex PDA unless the front cover lamp cover and flow cell cover are in place Flow cel
76. etector properties including the serial number firmware version and operating hours Monitoring of lamp properties including lamp ignitions lamp operation time and lamp intensity e Setting of limits for the lamp intensity and lamp operation time including display of warning messages when limits are exceeded e Reminders for service and qualification periods including display of warning messages when limits are exceeded 30 Doc 065378 01 1 12 Ze Description Leak detection e Wavelength verification System Wellness and Predictive Performance commands and parameters are available in the Chromeleon 7 Command window or the Chromeleon 6 8 Commands dialog box Doc 065378 01 1 12 31 Dionex PDA Operator s Manual 32 Doc 065378 01 1 12 3 e Operation and Maintenance 3 1 Getting Started 3 1 1 Initial Startup 1 If you are starting the Thermo Scientific Dionex ICS Series Photodiode Array Detector Dionex PDA for the first time press the main power switch on the rear panel see Figure 2 8 Press the power button on the front of the detector see Figure 2 1 After initial startup leave the main power switch on unless instructed to turn it off for example before performing a service procedure If the detector is installed with a Dionex ICS 5000 or Dionex ICS 3000 system use the power button on the front of the Dionex Dual Pump DP or Dionex Single Pump SP for routine on off control
77. example 1 0 Hz If any peaks of interest are less than a few seconds select a faster data collection rate for example 5 0 Hz If the data collection rate is too slow the start and end points of peaks are not accurately determined If the collection rate is too fast data files may occupy excessive disk space and post run analyses may require more processing time A slow data collection rate with a fast rise time may result in a longer system response than indicated by the rise time For example a data collection rate of 0 5 Hz and a rise time of 0 5 second results in a system response longer than 2 0 seconds At a data collection rate of 20 Hz the 3D sample wavelength range must be 310 nm Regardless of the data collection rate the reference wavelength if set must always be within the 3D range These are the recommended pairings for the rise time and data collection rate Rise Time Data Collection Rate seconds Hz 0 05 20 0 0 1 20 0 0 2 10 0 0 5 5 0 1 0 2 0 2 0 1 0 5 0 0 5 Doc 065378 01 1 12 45 Dionex PDA Operator s Manual Sample Wavelength The Dionex PDA measures absorbance over all wavelengths from 190 to 800 nm The deuterium lamp optimizes the UV range 190 to 380 nm while the tungsten lamp optimizes the visible range 380 to 800 nm Set the sample wavelength at the wavelength with the absorbance maxima for the analytes of interest When the analyte wavelength maxima are known the Dio
78. f the Dionex PDA in a manner not specified by Thermo Fisher Scientific may result in personal injury If there is a question regarding appropriate usage contact Technical Support for Dionex products In the U S and Canada call 1 800 346 6390 Outside the U S and Canada call the nearest Thermo Fisher Scientific office 1 4 1 Safety Messages and Notes This manual contains warnings and precautionary statements that can prevent personal injury and or damage to the Dionex PDA when properly followed Safety messages appear in bold type and are accompanied by icons as shown below VAN Indicates an imminently hazardous situation which if not avoided will result in death or serious injury DANGER Indicates a potentially hazardous situation which if avoided may result in death or serious injury WARNING VAN Indicates a potentially hazardous situation which if not avoided may result in minor or moderate injury CAUTION Indicates that the function or process of the instrument may be IMPORTANT e impaired Operation does not constitute hazard Messages d avertissement en frangais Signale une situation de danger imm diat qui si elle n est pas vit e entrainera des blessures graves a morielles gt DANGER Doc 065378 01 1 12 7 Dionex PDA Operator s Manual Signale une situation de danger potentiel qui si elle n est pas vit e pourrait entrainer des blessures graves a mortelles
79. filter paddle and is focused into the slit The light then passes through the slit to the grating where it is diffracted into the component wavelengths Measurement of the light occurs at the photodiode array Each diode measures a narrow portion of the spectrum Visible Focus Lens Tungsten Lamp ca Deuterium Lamp EM Flow Cell 4 Filter Paddle 7 Photodiode Array V e n R i Source Lens f n Spectrograph Lens MZ Ke e ei Wage Grating sl it Figure 2 4 Dionex PDA Optical System 14 Doc 065378 01 1 12 2 Description Optical System Component Tungsten Lamp Visible Focus Lens Deuterium Lamp Source Lens Flow Cell Spectrograph Lens Filter Paddle Slit Grating Photodiode Array Function The light source for visible and near infrared wavelengths 380 to 800 nm The tungsten lamp is focused through an opening in the internal structure of the deuterium lamp this allows the lamps to share the optical axis to the source lens Focuses the visible light from the tungsten lamp to the through hole of the deuterium lamp The light source for UV wavelengths 190 to 380 nm Receives the light from the tungsten and deuterium lamps and focuses it so that the beam passes through the flow cell The measurement site for sample absorbance The cell has a flat window on each side Thermo Fisher Scientific offers five cells for use with
80. gth Incorrect sample wavelength selected If little is known about the analytes in the sample collect spectra over the full wavelength range using both lamps For guidelines to follow when selecting the sample wavelength see page 47 84 Doc 065378 01 1 12 4 Troubleshooting Incorrect reference wavelength selected Select a different reference wavelength For guidelines to follow when selecting the reference wavelength see page 48 Bandwidth too wide Select a bandwidth that provides the resolution required to achieve the desired sensitivity Narrow spectra peaks require narrow bandwidths A wider bandwidth reduces baseline noise but may reduce peak height Reference bandwidth too wide Select a bandwidth that provides the resolution required to achieve the desired sensitivity A wider bandwidth reduces baseline noise but may increase the chance that the sample absorbs in the reference bandwidth thus causing reduced sensitivity and peak height Cell flow is reversed Check that the flow cell inlet tubing is routed through the heat exchanger see Figure 2 5 and is correctly connected to the inside front panel see Figure 5 1 Check that solvent flow is directed to the cell inlet and out the cell outlet Semi micro cell flow rate selected when standard cell is installed For operation at less than 1 0 mL min install a semi micro flow cell Doc 065378 01 1 12 85 Dionex PDA Operator s Manual
81. he Chromeleon 6 8 Client 1 Start the Chromeleon server if it is not already running If the Chromeleon server icon on the taskbar is crossed out in red amp server is not running To start the server right click the icon and select Start Server When the server is running and data acquisition is not occurring the icon is gray 88 If the Server Monitor icon is not on the taskbar click Start on the taskbar and select All Programs gt Chromeleon gt Server Monitor Click Start to start the server 2 Start the Chromeleon 6 8 client a Click Start on the Windows taskbar and select All Programs gt Chromeleon gt Chromeleon Doc 065378 01 1 12 35 Dionex PDA Operator s Manual b Select View gt Default Panel Tabset or click the corresponding toolbar button EH to display the panel tabset c To display the Dionex PDA Control panel select the Dionex PDA tab on the panel tabset see Figure 3 1 Hi Panel Tabset1 e 93409 AM Manually acquired samples will be stored temporarily in sequence SEQ ACMADLER locafiSystem manual Do 3409 AM Chromeleon server version 6 80 SP1 Build 2234 RC 3 started serial number 48 2 24 10 AM TC TC 3000 Serial Demo Firmare Version 99 99 Mo 2410 AM Column A Chip card detected Q Column B Chip card detected Ce gt Connected Ref Wavelength Autozero RE Qv m ELI om Show Pot Show 34 Plo vta 20 0 yl from Pos 1
82. hemical compatibility 17 25 44 113 Corrosion 17 25 44 107 108 113 Metal leaching 17 25 44 108 113 See also Cells Stainless steel systems Passivation 56 Standard flow cells 15 Chemical compatibility 107 Flow rate range 16 Heat exchanger volume 16 Operating pressure 107 Optical path length 16 107 Replacement procedure 97 See also Cells Volume 16 107 Windows replacement 95 96 Windows replacement kit 95 Standby procedure 55 Status bar 11 Step 43 Definition 52 Guidelines for selecting 52 Selection by software 52 67 Step override 52 System equilibration 75 Using the Smart Startup feature 38 System Wellness 30 T Technical Support 7 59 91 Temperature ambient 105 Reference mode selection 48 Timebase connections 74 83 Troubleshooting Baseline drift 78 79 Baseline noise 75 77 Elution time is slow 75 Lamp does not light 73 PDA does not respond 74 Peak shape is poor 84 Peak size is too big or small 84 Spectra not collected 83 Spectral resolution is poor 83 USB communication problem 86 Wavelength calibration fails 80 Wavelength verification fails 82 TTL control 23 117 Installation 117 Pin assignments 118 Tubing connections 26 Maintenance 55 56 TUNGSTEN VIS LED LED is flashing 12 73 74 LED is lighted 12 Tungsten lamp 14 15 Calibration 80 Lamp does not light 73 Output waning 76 Part number 131 Power supply 21 Replacing 10
83. i preparative cell or below 3 million counts for a semi micro cell follow these steps a Check that the flange of the deuterium lamp is aligned with the two locating pins in the optical bench see Section 5 3 If the flange is aligned the lamp is defective and should be replaced see Section 5 7 b Ifthe error message appears again contact Thermo Fisher Scientific for assistance Filter paddle has malfunctioned Check the Chromeleon Audit Trail If the Filter wheel sensor could not detect blocked position or Filter wheel sensor could not detect open position message is displayed see page 66 for instructions Failure of an electronics component Turn off the Dionex PDA power and contact Thermo Fisher Scientific for assistance NOTE Do not attempt to service the Dionex PDA electronics components All repairs of the electronics components must be performed by Thermo Fisher Scientific personnel 4 8 Wavelength Calibration Fails Deuterium lamp may be defective If the DEUTERIUM UV LED is flashing rapidly or if the LED fails to light replace the deuterium lamp see Section 5 7 If the DEUTERIUM UV LED is lighted but is not flashing open the Dionex PDA Wellness panel and run the wavelength calibration and the wavelength verification test see Section 4 14 2 If the Dionex PDA fails these procedures remove the flow cell from the detector and repeat both 80 Doc 065378 01 1 12 4 Troublesh
84. id steps are 0 05 0 1 0 2 0 4 0 5 1 2 and A Leak sensor error Not enough light to perform operation Over temperature error PDA is running a calibration or diagnostic function Not ready to accept this command Default Severity See Level Error Abort Error Abort Warning Abort Error Error Error Warning Abort Abort Abort Warning Warning Abort Error Warning Warning Abort Error page 62 page 63 page 64 page 64 page 64 page 64 page 65 page 65 page 65 page 65 page 65 page 66 page 66 page 66 page 66 page 67 page 67 page 68 page 68 page 68 page 69 60 Doc 065378 01 1 12 4 Troubleshooting Dionex PDA Related Alarms and Error Conditions Default Severity See Level The minimum wavelength must be less than the Error page 69 maximum wavelength Min wavelength x max wavelength x The range of wavelength bunching is 1 to 25 nm Error page 69 The range of wavelengths is outside the 190 to 800 nm Error page 69 limit Wavelength x Bandwidth x UV lamp control circuitry error while lamp is off Abort page 72 UV lamp error or control circuitry error while lamp is on Abort page 70 UV lamp error Abort page 70 UV lamp error while attempting to turn off Abort page 70 UV lamp error while attempting to turn on Abort page 70 UV lamp failed to turn on for the required operation Abort page 70 Visible lamp control circuitry error while lamp is off Abo
85. iew of Dionex PDA operating features includes Description an introduction to the chromatography software Chromeleon required for detector control Chapter3 Instructions for routine Dionex PDA operation with Operation and Chromeleon and guidelines for optimizing Dionex PDA Maintenance performance Preventive maintenance procedures Chapter 4 Minor problems that may occur during operation with Troubleshooting step by step procedures for how to isolate and eliminate the cause of each problem A list of Chromeleon Audit Trail error messages with an explanation of the possible cause of each message and the corrective action to take Chapter 5 Step by step instructions for routine service and parts Service replacement procedures the user can perform for the Dionex PDA Appendix A Specifications and installation site requirements for the Specifications Dionex PDA Appendix B Installation instructions for the Dionex PDA Installation Appendix C Spare parts for the Dionex PDA Reordering Information 6 Doc 065378 01 1 12 1 Introduction 1 A Safety and Regulatory Information The Dionex PDA was manufactured by Thermo Fisher Scientific at the following location 527 Lakeside Drive Sunnyvale CA 94088 3603 U S A The Dionex PDA is designed for use with IC ion chromatography BioLC biocompatible liquid chromatography and HPLC high performance liquid chromatography systems and should not be used for any other purpose Operation o
86. impurities Prepare all mobile phases and reagents with spectro grade solvents reagent grade chemicals and ASTM Type I or better filtered deionized water that meets the specifications in Table B 1 Leaking fittings Locate the source of the leak and tighten or replace the liquid line connection For tightening requirements refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Thermo Scientific Reference Library DVD P N 053891 Insufficient time for system equilibration after turning on lamp s or after changing mobile phase strength or composition The lamps usually require 20 to 30 minutes to stabilize For sensitive applications work or for detector validation allow at least 2 hours for the lamps to stabilize After installing a new lamp allow from 8 to 24 hours for the lamp to stabilize After changing mobile phases allow 20 to 30 column volumes for the system to stabilize Strongly retained components from previous analysis are slowly eluting To elute strongly retained species use a stronger mobile phase Re equilibrate with the standard mobile phase before resuming routine operation Clean the column as instructed in the column manual If the problem persists refer to the column manual for troubleshooting guidance Plot scale exaggerates baseline noise If autoscale is selected even a plot with low noise may fill the screen Check the Y axis scale values Air bubbles
87. in flow cell Remove the trapped air see Section 5 3 To prevent air from becoming trapped in the cell again follow these steps e Degas mobile phases and post column reagents by vacuum degassing or sparging with helium Doc 065378 01 1 12 75 Dionex PDA Operator s Manual e Connect a backpressure line to the cell see Section B 3 This increases the backpressure on the cell thereby shrinking bubbles and allowing them to pass more easily through the cell Contaminants in flow cell Clean the cell see Section 5 2 Incorrect lamp selected If a UV wavelength is selected make sure the deuterium lamp is on If a visible wavelength is selected make sure the tungsten lamp is on When a lamp is on the corresponding LED DEUTERIUM UV or TUNGSTEN VIS is lighted Lamp needs replacement The light output of the lamp decreases over time The lower light output may increase noise above an acceptable level especially if the lamp has been in service for more than 2000 hours If this occurs replace the lamp See Section 5 7 or Section 5 8 for instructions on replacing the deuterium lamp or tungsten lamp respectively Lamp incorrectly installed Make sure that both lamps are fully seated in the optical bench See Section 5 7 or Section 5 8 for installation instructions for the deuterium lamp or tungsten lamp respectively Inappropriate reference wavelength Select a reference wavelength in a quiet area of the spectrum
88. ine disruptions High sensitivity applications require a smooth low pulsation pump pressure output To ensure optimal results follow the maintenance schedule recommended in the pump user s manual All materials in the solvent delivery system must be fully compatible with the mobile phases required for the analysis For example IC and BioLC analyses frequently use mobile phases with extreme pH levels or high salt concentrations A PEEK pumping system and PEEK flow cell are required when running these mobile phases because the presence of stainless steel in the flow path would contaminate the system Reversed phase solvents methanol moderate concentrations of acetonitrile etc are acceptable for a PEEK system Other solvents and high concentrations of acetonitrile require a stainless steel system All tubing connections should be PTFE polytetrafluoroethylene Tefzel PEEK stainless steel or titanium as required for the specific operating pressures and application All mobile phase reservoirs should be compatible with the solvents used with your application Some plasticizers in blow molded components leach and are strong UV absorbers Cleanliness is very important After operating in detection modes that do not require optically clean reagents such as conductivity the solvent delivery system may need to be thoroughly cleaned A basic cleaning procedure is described below for additional information refer to the pump user
89. isolate the cause of the problem IMPORTANT Substituting non Dionex Thermo Scientific parts may impair the 5 1 performance of the Dionex PDA thereby voiding the product warranty Refer to the warranty statement in the Dionex Terms and Conditions for more information Liquid Leaks The Dionex PDA is plumbed with the parts listed below For tightening requirements refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Thermo Scientific Reference Library DVD P N 053891 Note that the tubing connected to the heat exchangers standard and semi micro cells only as well as the semi preparative cell inlet and outlet tubing cannot be replaced If a leak at the cell inlet for example cannot be eliminated by tightening the fitting you must replace the entire cell see Section 5 6 Table 5 2 Dionex PDA with Standard Cell Component PEEK Cell SST Cell Cell inlet tubing 0 38 mm 0 015 in ID P N 057304 N A Cell outlet tubing 0 38 mm 0 015 in ID P N 057304 N A Doc 065378 01 1 12 91 Dionex PDA Operator s Manual Table 5 2 Dionex PDA with Standard Cell Continued Component PEEK Cell SST Cell Cell inlet tubing 0 25 mm 0 010 in ID N A P N 056124 Cell outlet tubing 0 25 mm 0 010 in ID N A P N 051650 Reducing union fittings P N 055903 P N 055902 Ferrules P N 043276 P N 010262 Nuts P N 043275 P N 010261 Table 5 3 Dionex PDA with Semi Micro Cell Component PEEK Cell SST Ce
90. l grade tissue and go on to Step 11 If tightening the retaining nut s does not stop the leakage remove the window and inspect the O ring and groove for the cause of the leak fnecessary clean the groove and reinstall the O ring Dry the cell thoroughly with a lint free optical grade tissue and go on to Step 11 e Ifthe groove is scratched the cell must be replaced Contact Thermo Fisher Scientific to order a new cell Reinstall the flow cell in the optical bench 5 6 Replacing the Flow Cell Replace the flow cell if a colored substance stains the cell interior and cleaning the cell see Section 5 2 does not remove the stain or if excessive backpressure cracks the fused silica windows and you do not want to replace them see Section 5 5 1 2 Remove the flow cell from the optical bench see Section 5 4 Squeeze the handle of the new flow cell and insert it straight into the optical bench Release the handle and then pull it forward slightly If there is a click the cell is properly mounted If there is no click rotate the handle slightly just until the cell clicks into place Thread the flow cell inlet tubing through the tubing guide on the lamp cover and reinstall the tubing bracket see Figure 5 1 Thread the flow cell outlet tubing through the slot on the side of the flow cell cover Replace the cover and reconnect the cell inlet and outlet tubing Push the detector front cover into place Doc 065378
91. l heat exchanger not in place Check that the flow cell inlet tubing is threaded through the tubing guide on the lamp cover and secured in place with the tubing bracket see Figure 5 1 Lamp not stabilized or burned in The lamps usually require 20 to 30 minutes to stabilize For sensitive applications work or for detector validation allow at least 2 hours for the lamps to stabilize After installing a new lamp allow from 8 to 24 hours for the lamp to stabilize After changing mobile phases allow 20 to 30 column volumes for the system to stabilize Leaking flow cell Tighten fittings Also check that the backpressure on the cell does not exceed the specification see Section A 5 If the cell continues to leak replace it see Section 5 6 78 Doc 065378 01 1 12 4 Troubleshooting Absorbance in the reference wavelength Sample absorbance in the selected reference wavelength may cause excessive baseline drift Select a reference wavelength and reference bandwidth in an area of the spectrum where little absorption occurs see Reference Bandwidth on page 51 Thermo Fisher Scientific recommends selecting a reference wavelength i e active reference mode for gradient analyses and turning off the reference wavelength for isocratic analyses in a laboratory with a stable ambient temperature see Reference Wavelength on page 48 4 7 Deuterium Lamp Intensity Reading Too Low Light signal is not re
92. lacement instructions see Section 5 7 or Section 5 8 for the deuterium lamp or tungsten lamp respectively Doc 065378 01 1 12 57 Dionex PDA Operator s Manual 58 Doc 065378 01 1 12 4 1 4 Troubleshooting This chapter is a guide to troubleshooting problems that may occur while operating the Thermo Scientific Dionex ICS Series Photodiode Array Detector Dionex PDA e Section 4 1 describes error messages and how to troubleshoot them e Section 4 2 through Section 4 14 describe routine operating problems and how to resolve them e Section 4 14 2 describes some of the diagnostic features available in the Dionex PDA Moduleware and in Chromeleon chromatography software If you are unable to eliminate a problem contact Technical Support for Dionex products In the U S and Canada call 1 800 346 6390 Outside the U S and Canada call the nearest Thermo Fisher Scientific office Alarms and Error Conditions The Moduleware the instrument control firmware installed in the Dionex PDA periodically checks the status of certain system parameters If a problem is detected it is reported to Chromeleon and displayed in the Audit Trail Each error message is preceded by an icon that identifies the seriousness of the underlying problem see the table below You can change the severity level assigned to a problem whenever appropriate Icon Severity Level Description Warning A message is displayed in the Audit Trail
93. lays 1 and 2 can be configured in Chromeleon to switch any low voltage control The switched current must be less than 200 mA and 42 V peak H 5 Assignment Relay 1 output Relay 1 output Relay 2 output Relay 2 output TTL 1 output TTL 2 output TTL 1 input TTL 2 input TTL 3 input TTL 4 input TTL input or output DN E ra Ne TTL input or output Active Ground Active Ground Active Active Active Active Active Active Ground 1 Ground 2 B 7 Connecting to the Chromeleon PC B 7 1 Before You Begin Input Pin Function Autozero Reserved UV lamp on off Visible lamp on off Verify that the following tasks have been completed e Chromeleon 7 or Chromeleon 6 8 is installed on the computer The Chromeleon 7 or Chromeleon 6 8 license is installed NOTE Thermo Fisher Scientific strongly recommends installing Chromeleon before connecting the Dionex PDA to the computer When Chromeleon is installed first USB driver automatically information is loaded 118 Doc 065378 01 1 12 B Installation If installation is required follow the instructions in the appropriate installation guide The guides are provided on the Thermo Scientific Reference Library DVD P N 053891 e For Chromeleon 7 refer to Chromeleon 7 Installation Guide e For Chromeleon 6 8 refer to Installing the Chromeleon Chromatography Management System with a Dionex Ion Chromatograph
94. leaching Standard Flow Cell The standard flow cell assembly see Figure 2 5 is available in PEEK and 316 stainless steel Two built in heat exchangers one on the cell inlet tubing and one on the cell handle help stabilize the temperature of the mobile phase before it enters the cell The standard cell is designed for applications with 3 to 4 mm ID separator columns and flow rates of 0 5 to 5 0 mL min Reducing Union Fitting 5 5 Es Cell Outlet Tubing Wn Reducing Union Fitting o L 3 Heat Exchangers Spring Clip Figure 2 5 Standard Flow Cell Assembly Standard Cell Component PEEK Cell SST Cell Inlet tubing 0 38 mm 0 015 in ID P N 057304 N A Outlet tubing 0 38 mm 0 015 in ID P N 057304 N A Inlet tubing 0 25 mm 0 010 in ID N A P N 056124 Outlet tubing 0 25 mm 0 010 in ID N A P N 051650 Reducing union fitting P N 055903 P N 055902 Doc 065378 01 1 12 17 Dionex PDA Operator s Manual Semi Micro Flow Cell The semi micro flow cell assembly see Figure 2 6 is available in PEEK and 316 stainless steel Two built in heat exchangers one on the cell inlet tubing and one on the cell handle help stabilize the temperature of the mobile phase before it enters the cell The semi micro flow cell is designed for applications with 2 to 3 mm ID separator columns and flow rates up to 1 0 mL min i Cell Outlet Tubing Reducing Union Fitting
95. lear the ALARM LED In the Chromeleon 7 Command window see page 31 Click UV and then execute the ClearAlarmLED command In Chromeleon 6 8 click the Clear Alarm LED button on the Control panel or In the Commands dialog box see page 32 click UV and then execute the ClearAlarmLED command Lamp Does Not Light Lamp LED Is Flashing Rapidly Lamp default setting is not in effect When the factory default settings are in effect the deuterium and tungsten lamps turn on automatically each time the detector power is turned on If the required lamp does not turn on automatically you can turn it on from Chromeleon or the TTL input To restore the default setting for a lamp 1 Open the Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 2 Select UV and then execute the required command e UVLampPowerOnSetting for the deuterium lamp e VisLampPowerOnSetting for the tungsten lamp Lamp is old or burned out Replace the lamp See Section 5 7 or Section 5 8 for instructions on replacing the deuterium lamp or tungsten lamp respectively Doc 065378 01 1 12 73 Dionex PDA Operator s Manual 4 4 No Detector Response Detector power not on Check that the power cord is connected from the Dionex PDA rear panel to a power source Check that the main power switch on the rear panel is turned on Check the fuses and replace them if necessary see Section 5 9 Lamp not
96. lectrostatic discharge ESD handling procedures must be followed Ne retirez aucune des cartes lectroniques du d tecteur Aucun des composants sur les cartes ne peut tre r par par l utilisateur Toute r paration doit tre effectu e par un personnel qualifi utilisant des MISE EN GARDE proc dures correctes de d charge lectrostatique Halten Sie sich von der Elektronik des Dionex PDA fern Die Elektronik kann nicht vom Anwender gewartet werden Falls ein Service erforderlich ist ist dieser von qualifiziertem Personal durchzuf hren VORSICHT Dabei m ssen die geeigneten Verfahren zur elektrostatischen Entladung ESD eingehalten werden Power Supply The power supply module contains connections to the AC power source and provides regulated low voltage power for the Dionex PDA Power entry components are shielded and filtered to prevent electromagnetic interference EMI SHOCK AND FIRE HAZARD The power supply module operates at line potentials Refer all servicing to qualified personnel WARNING d alimentation lectrique fonctionne aux potentiels du secteur Faites DANGER D LECTROCUTION ET D INCENDIE Le module effectuer toutes les r parations par un personnel qualifi AVERTISSEMENT STROMSCHLAG UND BRANDGEFAHR Das Modul zur Stromversorgung wird mit Netzspannung betrieben Der Service darf nur von qualifiziertem Personal durchgef hrt werden WARNUNG 20 Doc 065378 01 1 12 Ze Descrip
97. led Run the wavelength calibration and wavelength verification test for the new lamp see Section 4 14 2 100 Doc 065378 01 1 12 5 Service 5 8 Replacing the Tungsten Lamp 1 Stop the Chromeleon instrument controller or server 2 Press the power button on the front of the Dionex PDA to turn off the power 3 Turn off the main power switch on the Dionex PDA rear panel The lamp housing and base may be hot to the touch especially after the lamp has been in operation for a long time Wait until the lamp has cooled down before continuing CAUTION La lampe et la base de la lampe peuvent tre chaudes au toucher particuli rement apres que la lampe a t allum e pendant longtemps Attendez que la lampe ait refroidi avant de continuer MISE EN GARDE Das Lampengehause und die Lampenbefestigung k nnen sehr hei werden besonders wenn die Lampe l ngere Zeit in Betrieb war Warten Sie bis die Lampe abgek hlt ist bevor Sie diese ber hren VORSICHT 4 Grasp the detector front cover by the sides and pull straight off to remove 5 Standard or semi micro cell Remove the tubing bracket from the lamp cover see Figure 5 1 6 Remove the flow cell inlet tubing from the tubing guide in the lamp cover see Figure 5 1 7 Remove the flow cell cover from the inside front panel see Figure 5 1 8 Move the flow cell tubing out of the way Remove the four screws holding the lamp cover in place and then remove the cover and set it a
98. ll Cell inlet tubing 0 12 mm 0 005 in ID P N 063897 N A Cell outlet tubing 0 38 mm 0 015 in ID P N 057304 N A Cell inlet tubing 0 12 mm 0 005 in ID N A P N 063903 Cell outlet tubing 0 25 mm 0 010 in ID N A P N 051650 Reducing union fittings P N 055903 P N 055902 Ferrules P N 043276 P N 010262 Nuts P N 043275 P N 010261 Table 5 4 Dionex PDA with Semi Preparative Cell Component PEEK Cell Cell inlet tubing 0 51 mm 0 020 in ID P N 042855 Cell outlet tubing 0 51 mm 0 020 in ID P N 042855 Union fittings P N 042627 Ferrules P N 043276 Nuts P N 043275 92 Doc 065378 01 1 12 5 Service 5 2 5 3 Cleaning the Flow Cell Film deposits on the flow cell windows may cause excessive baseline noise or high absorbance offset 1 Pump methanol through the cell for 20 to 30 minutes at 1 0 mL min 2 Pump deionized water through the cell for 20 to 30 minutes at 1 0 mL min If the procedure above does not clean the cell follow these steps 1 Disconnect the liquid lines from the cell in and out connections 2 Connect a luer adapter to the cell in connection 3 Using a syringe flush the cell with a succession of at least 10 uL each of deionized water acetone and 3 M HNO3 4 Reconnect the cell liquid lines Flush the cell with deionized water for 20 to 30 minutes at 1 0 mL min Removing Trapped Air from the Flow Cell Trapped air bubbles in the flow cell may cause pulsations of the baseline or random n
99. m 20 uL 0 5 to 5 0 mL min P N 056126 SEMI MICRO FLOW CELLS Cell Material Cell Cell Path Volume of Heat Intended Flow Volume Length Exchanger Rate Range Inlet Tubing PEEK 31uL 9mm 5 Up to 1 0 mL min P N 064169 316 stainless steel 3 1 uL 9mm 5 pL Up to 1 0 mL min P N 064168 SEMI PREPARATIVE FLOW CELL Cell Material Cell Cell Path Volume of Heat Intended Flow Volume Length Exchanger Rate Range Inlet Tubing PEEK 0 7 uL 0 4 mm N A 5 0 to P N 064167 100 0 mL min IMPORTANT Table 2 1 Dionex PDA Flow Cells Do not touch the cell windows If you touch a window clean it with isopropyl alcohol IPA and a clean lens tissue Strong bases can etch the fused silica windows of the flow cell If the mobile phase is a base make sure the mobile phase concentration does not exceed 0 1 M If the concentration of the base is greater than 50 mM disconnect the separator column and flush the system with deionized water for 5 minutes at 1 0 mL min immediately after the analysis If strong base remains in the cell for 1 to 2 days the cell windows may need to be replaced see Section 5 5 16 Doc 065378 01 1 12 Ze Description Do not use a PEEK flow cell with normal phase or chlorinated solvents these solvents will damage the cell Do not use a stainless steel flow cell with low pH solutions these solutions may cause corrosion contamination and metal
100. micro flow cell outlet tubing assembly Reducing union fitting PEEK Ferrule Nut Doc 065378 01 1 12 131 Dionex PDA Operator s Manual Part Number Item 060498 Dionex AD25 Dionex PDA Dionex PDA 100 Flow Cell Windows Replacement Kit Semi Micro Flow Cell 316 Stainless Steel 063884 Stainless steel semi micro flow cell with heat exchangers 051650 Stainless steel semi micro flow cell outlet tubing assembly 055902 Reducing union fitting stainless steel 010262 Ferrule 010261 Nut 060498 Dionex AD25 Dionex PDA Dionex PDA 100 Flow Cell Windows Replacement Kit Semi Preparative Flow Cell PEEK 064167 PEEK semi preparative flow cell 042855 PEEK semi preparative flow cell outlet tubing assembly 042627 Union fitting 043276 Ferrule 043275 Nut 132 Doc 065378 01 1 12 Numerics 2D data collection 1 3D Data Acquisition license 4 30 Error message 60 63 3D data collection 3D Data Acquisition license 4 30 Bunch width selection 51 Reducing data file size 53 Step time selection 52 A Absorbance calculation 51 Absorbance range 22 Achtung icon 8 Active reference mode 47 48 See also Reference wavelength Selecting 78 Turning off 48 Turning on 47 Air bubbles in cell Preventing 75 115 Removing 93 Air conditioning 48 ALARM LED Clearing the alarm 73 LED is lighted 12 13 73 Alarm LED Clearing the alarm 73 Ambient temperature fluctuations 48 Analog output connectors 2 21
101. n it off for example before performing a service procedure Use the power button on the front of the detector for routine on off control SHOCK HAZARD To avoid elecirical shock use a grounded receptacle Do not operate the Dionex PDA or connect it to AC power without an earthed ground connection WARNING The power supply cord is used as the main disconnect device Make sure the socket outlet is located near the Dionex PDA and is easily accessible CAUTION Doc 065378 01 1 12 23 Dionex PDA Operator s Manual Operation at AC input levels outside of the specified operating voltage range may damage the Dionex PDA gt CAUTION DANGER D ELECTROCUTION Pour viter toute lectrocution il faut utiliser une prise de courant avec prise de terre Ne l utilisez pas et ne le branchez pas au secteur C A sans utiliser de branchement mis a la AVERTISSEMENT terre gt Le cordon d alimentation principal est utilis comme dispositif principal de d branchement Veillez ce que la prise de base soit situ e install e pr s du module et facilement accessible gt MISE EN GARDE STROMSCHLAGGEFAHR Zur Vermeidung von elektrischen Schlagen ist eine geerdete Steckdose zu verwenden Das Ger t darf nicht ohne Erdung betrieben bzw an Wechselstrom angeschlossen WARNUNG werden gt Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung Stellen Sie sicher daB sich die Steckdose nahe am Gerat befindet un
102. nex PDA can run five separate wavelengths without the necessity for collecting spectra Collecting individual wavelengths instead of the spectra offers two advantages it uses less disk space and it eliminates the need to perform extractions for analyses that do not require spectral data If little is known about the analytes in the sample collect spectra over the full wavelength range using both lamps Although this requires more disk space it provides complete information about the analytes and the spectra can be used to determine peak identity purity and wavelength maxima Bandwidth The bandwidth defines a wavelength range around the wavelength at which the chromatogram is measured Increasing the bandwidth increases the number of different wavelength signals averaged at each point in time As the bandwidth increases baseline noise decreases however this may decrease the signal especially of those peaks that exhibit spectral peak maxima Select a bandwidth that provides the resolution required to achieve the desired sensitivity Selecting a wider bandwidth reduces baseline noise but may also reduce peak height For narrow spectral peaks select narrow bandwidths Example Chromatogram Selecting the Bandwidth Figure 3 6 illustrates how selecting a wide bandwidth for both the sample and reference wavelengths reduces noise by averaging over a wavelength range The operating conditions are Sample wavelength 254 nm Reference wa
103. ng Spring Fuse Holder Side View Insert screwdriver and twist to release each side Main Power Receptacle Figure 5 4 Main Power Fuse Holder Doc 065378 01 1 12 103 Dionex PDA Operator s Manual 5 Replace the two fuses in the holder with new 4 0 amp fast blow IEC 127 fuses P N 954763 Thermo Fisher Scientific recommends always replacing both fuses 6 Reinsert the fuse holder into the compartment The fuse holder is keyed to fit only in the correct orientation Apply pressure evenly against the holder until the locks are engaged When correctly installed the fuse holder is flush against the rear panel 7 Reconnect the power cord and turn on the power 104 Doc 065378 01 1 12 A Specifications A 1 Electrical Main Power 85 to 265 VAC 47 to 63 Hz auto sensing no manual adjustment required Typical input power 100 W Maximum line draw 3 5 A at 110 VAC at power up Fuses Two fast blow IEC 127 fuses P N 954763 rated at 4 0 A A 2 Physical Dimensions Height 17 4 cm 6 8 in Width 44 4 cm 17 5 in Depth 50 3 cm 19 8 in Clearance required behind detector 6 cm 2 4 in Weight 18 1 kg 40 Ibs A 3 Environmental Operating 4 to 40 C 40 to 104 F constant temperature Temperature Operating 5 to 95 relative humidity noncondensing Humidity Doc 065378 01 1 12 105 Dionex PDA Operator s Manual AA Detector Optical System Light Sources
104. oise and low readings Flush the cell with methanol for 20 minutes If this does not remove the trapped air follow these steps 1 Disconnect the waste line from the cell Also disconnect the backpressure device 2 Using a small syringe push 3 to 5 mL of methanol through the cell Or bypass the column and pump methanol through the system at 1 0 mL min 3 Reconnect the waste line and backpressure device Doc 065378 01 1 12 93 Dionex PDA Operator s Manual 5 4 Removing the Flow Cell from the Optical Bench The flow cell must be removed from the optical bench in order to inspect the cell for leaks or obstructions replace the cell windows see Section 5 5 or install a new cell see Section 5 6 1 Grasp the Dionex PDA front cover by the sides and pull straight off to remove Disconnect the tubing connected to the flow cell inlet and outlet see Figure 5 1 Remove the flow cell cover from the inside front panel see Figure 2 3 Standard or semi micro cell Remove the tubing bracket from the lamp cover see Figure 5 1 Remove the flow cell inlet tubing from the tubing guide in the lamp cover see Figure 5 1 Squeeze the handle of the flow cell and pull it out of the optical bench Cell Inlet ur q Jw Figure 5 1 Removing the Flow Cell from the Optical Bench Flow cell cover not shown 94 Doc 065378 01 1 12 5 Service 5 5 Replacing the Flow Cell Windows Contamina
105. om Chromeleon or the TTL input If you recently installed a new deuterium lamp check that the UV lamp connector wires are routed through the wire guide in the optical bench see Figure 5 3 and are not pinched under the lamp cover Check the number of hours the lamp has been in service Open the Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 and then select UV If the error message relates to the deuterium lamp execute the UVLampAge command 70 Doc 065378 01 1 12 4 Troubleshooting If the deuterium lamp has been in operation for more than 2000 hours replace it see Section 5 7 If the error message appears again contact Thermo Fisher Scientific for assistance If the deuterium lamp has been in operation for ess than 2000 hours turn off the lamp for at least 3 minutes and then turn it on again If the error message reappears replace the lamp see Section 5 7 If the error message does not appear again run a manual data acquisition for about 30 minutes If you notice a shift in the absorbance signal during this time replace the lamp If the error message relates to the tungsten lamp execute the VisLampAge command If the tungsten lamp has been in operation for more than 2000 hours replace it see Section 5 8 If the error message appears again contact Thermo Fisher Scientific for assistance If the tungsten lamp has been in operation for ess than 2000
106. ooting procedures If the detector fails the wavelength calibration again contact Thermo Fisher Scientific for assistance e Deuterium lamp intensity out of calibration 1 2 Remove the cell from the optical bench see Section 5 4 Check the deuterium lamp intensity a b Open the Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 Select UV and then select LampIntensity If the lamp intensity reading is above 10 million counts for a standard or semi preparative cell or above 3 million counts for a semi micro cell follow these steps a Open the Chromeleon 7 Command window see page 31 or the Chromeleon 6 8 Commands dialog box see page 32 Select UV and then select UV_Calibration Execute the Intensity command to calibrate the lamp intensity Execute the Autozero command to run the autozero routine If no error message is displayed flush the cell with the mobile phase for the application and or clean the cell as instructed in Section 5 2 Reinstall the cell in the optical bench Autozero the detector again to verify that the problem has been resolved If the error message appears again contact Thermo Fisher Scientific for assistance If the lamp intensity reading is below 10 million counts for a standard or semi preparative cell or below 3 million counts for a semi micro cell follow these steps a Check that the flange of the deuterium lamp is
107. ough the slot on the right side 12 Push the detector front cover into place 13 Connect the cell inlet tubing to the separator column outlet Doc 065378 01 1 12 115 Dionex PDA Operator s Manual B 4 Connecting the Waste Line Connect the waste line P N 055075 to the Dionex PDA rear panel see Figure B 3 Place the free end of the waste line in a waste container below the level of the workbench on which the Dionex PDA is installed IMPORTANT The drain tube must remain below the drain port If the drain tube is above the drain port the drip tray may overflow inside the detector Analog Outputs 4 Drain Tube Connector Relay TTL Connectors USB Connector Fuse Holder 0606 6 Power Entry B 5 Figure B 3 Dionex PDA Rear Panel Connecting the Analog Outputs Optional Connect a recorder an integrator or an A D data acquisition device to the ANALOG OUT connector on the Dionex PDA rear panel see Figure B 3 The four Dionex PDA analog outputs provide a 1 volt output maximum The outputs are controlled by absorbance wavelengths 1 through 4 in Chromeleon The chromatography software controls the wavelength sample bandwidth reference wavelength full scale absorbance output and offset within the 0 to 1 volt range 116 Doc 065378 01 1 12 B Installation B 6 Connecting the Relays TTLs Optional gt CAUTION gt WARNING gt AVERTISSEMENT
108. r power is initially turned on the lamp age already indicates some elapsed time this is the time that was required for factory calibration and test procedures Doc 065378 01 1 12 87 Dionex PDA Operator s Manual Wavelength calibration Purpose Improves wavelength accuracy in the UV range by reassigning new wavelengths to each pixel based on the emission spectrum from the deuterium lamp The detector will perform the wavelength calibration routine and upload the result pass or fail to Chromeleon The results of both the initial calibration and the last calibration are stored in the calibration log You can view the results at any time In Chromeleon 7 a Verify the following conditions no solvent is flowing through the cell the background absorbance is low and there are no bubbles in the light path b Open the Command window see page 39 select UV and execute the Wavelength Calibration command In Chromeleon 6 8 a Verify the following conditions no solvent is flowing through the cell the background absorbance is low and there are no bubbles in the light path b To open the Wellness panel click the Wellness button on the Dionex PDA Control panel c Click the wavelength script button under Calibration Wavelength verification Purpose Tests the accuracy of the selected wavelength The accuracy is verified for the following wavelengths 360 9 418 8 and 536 5 The results of the test pass or
109. r rise time allows more averaging of the signal and results in less short term noise see Figure 3 5 However a rise time that is too long may result in reduced peak heights and asymmetric peak shapes When set correctly the rise time significantly reduces baseline noise but reduces peak height only slightly 0 0250 m Rise Time 0 5 sec Baseline Noise 22 AU 04 J i b WVL 254 du TN Tm 0 0100 T 0 00 0 0150 2 00 5 00 Rise Time 2 0 sec Baseline Noise 10 AU 0 0000 1 0 0100 1 0 0200 WVL 254 nm i N mu UNI Ji WW NW p UM SEE 0 00 1 00 Figure 3 5 Effect of Rise Time on Baseline Noise 44 Doc 065378 01 1 12 3 Operation and Maintenance Data Collection Rate The data collection rate or sample rate is the number of data points per second Hz at which the computer stores data from the Dionex PDA The detector electronics collect data at up to 20 0 Hz The Dionex PDA data collection rate settings are 0 25 0 5 1 0 2 0 2 5 default 5 0 10 0 or 20 0 Hz The maximum number of data points is stored at 20 0 Hz In general each peak should be defined by at least 20 data points For chromatograms with co eluting peaks or low signal to noise ratios 40 data points per peak is recommended If all peaks are relatively wide select a slower data collection rate for
110. rt page 72 Visible lamp error or control circuitry error while lamp is Abort page 70 on Visible lamp error Abort page 70 Visible lamp error while attempting to turn off Abort page 72 Visible lamp error while attempting to turn on Abort page 70 When collecting at 20 Hz the spectrum range cannot be Abort page 72 more than 310 nm Please lower the data rate or narrow the spectrum range Doc 065378 01 1 12 61 Dionex PDA Operator s Manual 3DFIELD RefWavelength and or RefBandwidth is out of A range To troubleshoot For all data collection rates other than 20 Hz select parameters that meet the following criteria 190 lt A T lt 800 Where Reference wavelength BW Reference bandwidth For example the following parameters are VALID Wavelength 190 to 800 nm Reference wavelength 750 nm Reference bandwidth 50 nm These parameters are valid because 750 nm 25 nm 50 of 50 nm 775 nm which is less than 800 nm The following parameters are NOT VALID Wavelength 190 to 600 nm Reference wavelength 750 nm Reference bandwidth 50 nm These parameters are invalid because 750 nm 25 nm 50 of 50 nm 775 nm which is greater than 600 nm 62 Doc 065378 01 1 12 4 Troubleshooting When the data collection rate is 20 Hz select parameters that meet the following criteria Minimum A lt K lt Maximum A Maximum Minimum A lt 310 nm Where Reference wavelength
111. s manual for an explanation of the hazard and how to proceed GC Declaration of Conformity The TUV GS C US Mark safety label and the CE Mark label on the Dionex PDA indicate that the Dionex PDA is in compliance with the following standards EN 61010 1 2001 safety CAN CSA C22 2 No 1010 1 92 A2 97 safety UL 61010C 1 2002 R8 02 safety and EN 61326 1997 A1 1998 EMC susceptibility and immunity Doc 065378 01 1 12 Dionex PDA Operator s Manual 10 Doc 065378 01 1 12 2 Description 2 1 Front Features Figure 2 1 illustrates the features on the front of the Thermo Scientific Dionex ICS Series Photodiode Array Detector Dionex PDA Status Bar Power Button Front Cover Figure 2 1 Dionex PDA Front Features e The status bar provides LEDs light emitting diodes that indicate the status of several Dionex PDA components and functions see Figure 2 2 e Use the power button for routine on off control of the Dionex PDA NOTE The main power switch is on the Dionex PDA rear panel see Figure 2 8 Always leave the main power switch on unless instructed to turn it off for example before performing a service procedure e The front cover provides access to the components inside the Dionex PDA To remove the cover grasp the cover by the sides and pull it straight off Doc 065378 01 1 12 11 Dionex PDA Operator s Manual CONNECTED ALARM DEUTERIUM UV
112. s the reference intensity When running an isocratic analysis in a laboratory with stable ambient temperature operating the detector with the active reference mode turned off ensures the lowest baseline noise It also ensures that fluctuations in signal intensity in the reference wavelength do not cause additional noise NOTE When you enter Off as the reference wavelength setting the reference bandwidth is not used The reference value is the first data point of the sample wavelength and bandwidth after autozero Example Chromatogram Selecting the Reference Wavelength Figure 3 7 shows the results obtained from two different channels within the same run When the reference wavelength mode is Off 1 the active reference mode is cancelled the baseline drift is 120 iL AU hour When the active reference mode is selected the baseline drift is reduced to 40 n AU hour 48 Doc 065378 01 1 12 3 e Operation and Maintenance The operating conditions are Sample wavelength 520 nm Bandwidth 10 nm Reference bandwidth 50 nm active reference mode only Flowing water at 1 0 mL min 10 35 MPa 1500 psi Reference Wavelength Mode Off Baseline Drift 120 AU hour mAU min Reference Wavelength Mode Active Baseline Drift 40 AU hour mAU Figure 3 7 Effect of Reference Wavelength on Baseline Drift Doc 065378 01 1 12 49 Dionex PDA Operator s Manual Ref
113. see Figure 5 1 4 Squeeze the handle of the flow cell and insert it straight into the optical bench Release the handle and then pull it forward slightly If there is a click the cell is properly mounted If there is no click rotate the handle slightly just until the cell clicks into place 5 Thread the flow cell inlet tubing through the tubing guide on the lamp cover and reinstall the tubing bracket see Figure 5 1 6 Thread the flow cell outlet tubing through the slot on the side of the flow cell cover Replace the cover and reconnect the cell inlet and outlet tubing 7 Standard or semi micro cell Connect the cell inlet tubing to the reducing union fitting P N 055903 for a PEEK cell P N 055902 for a stainless steel cell on the heat exchanger tubing see Figure B 1 Doc 065378 01 1 12 113 Dionex PDA Operator s Manual d Cell Outlet Tubing Reducing Union Fitting 55 5 PEEK cell P N 055903 Stainless steel cell P N 055902 Reducing Union Fitting 3 PEEK cell P N 055903 Stainless steel cell P N 055902 E ir Y k Ier Flow Cell I Heat Exchangers 7 Spring Clip Figure B 1 Standard or Semi Micro Flow Cell Connections 8 Semi preparative cell Connect the cell inlet tubing to a union fitting P N 042627 see Figure B 2 Cell Outlet Tubing 0 51 mm 0 020 in ID Union Fitting P N 042855 P N 042627 Union Fitting a P N 042627 A Cell
114. seline 78 4 7 Deuterium Lamp Intensity Reading Too 79 4 8 Wavelength Calibration Fails 80 4 9 Wavelength Verification 82 4 10 No Spectra Collected orur taria ena a eee 83 4 11 Low Spectral Resolution 83 4 12 Peaks Too Large or Small 84 4 13 Poor Peak Shape m reei eee Ree ERE 84 4 14 Faulty USB Communication 86 4 14 1 Moduleware Run Time Diagnostics 87 4 14 2 Software Diagnostics and Calibration 87 5 s SEVICE Zeta 91 5 1 Ligua Leaks ein e ae ele be EE AE ay EE 91 5 2 Cleaning the Flow Cell 0 eee eee 93 5 3 Removing Trapped Air from the Flow Cell 93 5 4 Removing the Flow Cell from the Optical Bench 94 5 5 Replacing the Flow Cell Windows 95 5 6 Replacing the Flow Cell 97 5 7 Replacing the Deuterium 98 5 8 Replacing the Tungsten 101 5 9 Replacing the Main Power Fuses 103 Doc 065378 01 1 12 iii Dionex PDA Operator s Manual A Specifications 105 AW i iie dm ets p
115. service procedure Use the power button on the front of the Dionex PDA for routine on off control 4 For Windows Vista Windows Vista detects the Dionex PDA and performs the USB driver installation a When the driver installation is complete the Chromeleon USB Auto Configuration Wizard automatically appears Accept the default option for Chromeleon 7 Create a new instrument or Chromeleon 6 8 Create a new timebase and click OK This opens the Auto Configuration dialog box Leave the dialog box open b Goon to Section B 10 5 For Windows XP Windows XP detects the Dionex PDAand launches the Found New Hardware Wizard Use the wizard to install the Dionex PDA as described below a Ifasked whether Windows can connect to Windows Update to search for software select No not this time b Accept the default option Install the software automatically and click Next c When the hardware wizard reports that the software for the detector has been installed click Finish 124 Doc 065378 01 1 12 B Installation d The Chromeleon USB Auto Configuration Wizard automatically appears Accept the default option for Chromeleon 7 Create a new instrument or Chromeleon 6 8 Create a new timebase and click OK This opens the Auto Configuration dialog box Leave the dialog box open e Goon to Section B 10 NOTE If Windows fails to detect the Dionex PDA refer to Section 4 14 for corrective action B 10 Configuring the
116. sibility and will not be liable for any errors omissions damage or loss that might result from any use of this document even if the information in the document is followed properly Revision history Revision 01 released January 2012 For Research Use Only Not for use in diagnostic procedures Contents 1 Introduction Ll Detector Overview cc ede eR ee teed ded aed 1 1 2 Theory of Photodiode Array Detection 2 1 2 1 Advantages of Photodiode Array Detection 3 1 3 Operator s Manual Overview 6 1 4 Safety and Regulatory Information 7 1 4 1 Safety Messages and Notes 7 1 4 2 Safety Labels eng eco ee ee oe cae wears 9 1 4 3 Declaration of Conformity 9 2 11 2 1 Front Features KENNEN E E E E EE ge PE 11 2 4 Inside Front Panels tea NEE te aes A 13 2 3 Optical NEE ee ee seg ER SE EA a adeo rae 14 2 3 1 Blow Cells iiir Dx ur n RR IRE E RED 16 24 Electronics vac lese lise edad RR TA 20 2 5 RearPatel i e sod ELDER edu CERE EK RE E 22 2 6 Operating 25 2 6 1 Mobile Phases eer er gee aed 25 2 6 2 Solvent Delivery System 26 Doc 065378 01 1 12 i Dionex PDA Operator s
117. side 9 Squeeze the clip on the visible lamp connector and disconnect it from the 4 pin bulkhead connector on the side wall see Figure 5 3 10 Use a screwdriver to loosen the tungsten lamp screws and then pull the mounting assembly away from the optical bench NOTE The screws are captive in the lamp base and do not need to be removed 11 Inspect the new tungsten lamp P N 056123T for fingerprints and dust If necessary clean the lamp with IPA isopropyl alcohol Doc 065378 01 1 12 101 Dionex PDA Operator s Manual 12 Carefully insert the new lamp into the optical bench and tighten the three screws that secure the lamp to the optical bench The replacement lamp is pre aligned in the mount IMPORTANT To ensure proper performance the lamp must be fully seated 13 Squeeze the clip on the Vis lamp connector and insert it into the 4 pin bulkhead connector on the side wall Route the wires through the wire guide in the optical bench see Figure 5 3 14 Replace the lamp cover IMPORTANT Do not pinch the Vis lamp connector wires under the lamp cover 15 Thread the cell inlet tubing through the tubing guide on the lamp cover and reinstall the tubing bracket 16 Replace the flow cell cover and reconnect the inlet and outlet tubing IMPORTANT Do not pinch the tubing under the flow cell cover 17 Replace the detector front cover 18 Turn on the detector power 19 Start the Chromeleon instrument controller or s
118. tector Shut down the Chromeleon instrument controller or server and turn off the Dionex PDA power wait 30 seconds and then power up both the instrument controller or server and the detector If the error message appears again contact Thermo Fisher Scientific for assistance Doc 065378 01 1 12 65 Dionex PDA Operator s Manual Diagnostic is running To troubleshoot This message appears if you attempt to issue a command or select a parameter while a diagnostic routine is running Wait until the diagnostic routine is completed before making any changes DSP communication failure To troubleshoot This message appears if there is a communication failure between the DSP digital signal processor and the CPU Turn off the Dionex PDA power for 30 seconds and then turn it on again If the error message appears again contact Thermo Fisher Scientific for assistance Filter wheel sensor could not detect blocked position Filter wheel sensor could not detect open position A backup paddle alignment routine ensures that the Dionex PDA remains functional even if the sensor cannot detect the filter wheel position Thus if this is the only error reported you may continue operation and defer troubleshooting To troubleshoot 1 Turn off the Dionex PDA power for 30 seconds and then turn it on again 2 Ifthe error message appears again check the deuterium lamp intensity a Open the Chromeleon 7 Command window
119. tector front cover by the sides and pull straight off to remove Standard or semi micro cell Remove the tubing bracket from the lamp cover see Figure 5 1 Remove the flow cell inlet tubing from the tubing guide in the lamp cover see Figure 5 1 Remove the flow cell cover from the inside front panel see Figure 5 1 Move the flow cell tubing out of the way Remove the four screws holding the lamp cover in place and then remove the cover and set it aside 98 Doc 065378 01 1 12 5 Service 9 Squeeze the clip on the UV lamp connector and disconnect it from the 6 pin bulkhead connector on the side wall see Figure 5 3 Flow Cell Cover Deuterium Screw Lamp ec Mire Guide UV Lamp Connector 2 lt 6 pin Bulkhead Connector 4 4 Bulkhead Connector Locating Tungsten Visible Lamp Connector Pin Red Power Lead Lamp Leak Sensor Figure 5 3 Lamp Connections 10 Loosen the three screws in the deuterium lamp flange see Figure 5 3 and pull the lamp out of the optical bench NOTE The screws are captive in the lamp base and do not need to be removed 11 Inspect the new deuterium lamp P N 939016T for fingerprints and dust If necessary clean the lamp with IPA isopropyl alcohol 12 Line up the
120. ted flow cell windows can significantly increase baseline noise and cause wavelength calibration to fail If cleaning the cell see Section 5 2 does not eliminate these problems replace both windows NOTE The windows in the semi preparative flow cell cannot be replaced If cleaning the windows does not eliminate the problems described above order a new semi preparative cell The Dionex AD25 Dionex PDA Dionex PDA 100 Flow Cell Windows Replacement Kit P N 060498 contains all of the parts required to replace the fused silica windows in a standard or semi micro cell The kit is optional and must be ordered separately from the Dionex PDA 1 Remove the flow cell from the optical bench see Section 5 4 and place the cell on a clean work surface Disassembling the cell with bare hands may introduce contaminants into the system Before proceeding put on a pair of latex gloves that are lint free particle free and oil free IMPORTANT Even minute particles of dust dirt etc on the flow cell parts can contaminate the cell and result in excessive baseline noise and drift Using the windows replacement tool P N 060497 remove one of the flow cell retaining nuts from the cell see Figure 5 2 It does not matter which retaining nut is removed first Remove and discard the old window Use tweezers to carefully remove the O ring from the groove see Figure 5 2 Do not scratch the groove The following factors will prevent the new
121. terre Ne l utilisez pas et ne le branchez pas au secteur sans utiliser de branchement mis la AVERTISSEMENT terre gt Le cordon d alimentation principal est utilis comme dispositif principal de d branchement Veillez ce que la prise de base soit situ e install e pr s du module et facilement accessible gt MISE EN GARDE STROMSCHLAGGEFAHR Zur Vermeidung von elektrischen Schlagen ist eine geerdete Steckdose zu verwenden Das Ger t darf nicht ohne Erdung betrieben bzw an Wechselstrom angeschlossen WARNUNG Werden gt Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung Stellen Sie sicher daB sich die Steckdose nahe am Gerat befindet und leicht zuganglich ist gt VORSICHT Doc 065378 01 1 12 123 Dionex PDA Operator s Manual B 9 Installing the USB Device Drivers 1 Turn on the computer power 2 Log onto Windows Vista or Windows XP as an administrator For a network computer log on as a user with local computer administrator privileges IMPORTANT Before turning on the Dionex PDA power verify that Chromeleon is installed on the PC and the license code was entered see Section B 7 1 If the chromatography software is not installed first Windows will be unable to identify the detector 3 Turn on the main power switch on the rear panel of the Dionex PDA NOTE Always leave the main power switch on unless instructed to turn it off for example before performing a
122. the Dionex PDA standard cells in both PEEK and 316 stainless steel semi micro cells in both PEEK and 316 stainless steel and semi preparative cells in PEEK only Receives the light from the flow cell and focuses it onto the slit The motorized filter paddle in the spectrograph has three positions e Open Light passes unobstructed along the light path when the holmium oxide filter is moved out of the light path e Blocked No light passes along the light path used to measure the dark signal without turning off the lamps e Holmium Places the holmium oxide filter in the light path used to verify wavelength accuracy The width of the slit equivalent to 1 nm optimizes the optical resolution Diffracts the light beam into its component wavelengths and directs the light onto the photodiode array A series of 1024 photosensitive elements Each element measures a narrow band of the spectrum A spectrum is obtained by measuring the light intensity of each wavelength and reporting the results over the selected wavelength range Doc 065378 01 1 12 15 Dionex PDA Operator s Manual 2 3 1 Flow Cells Table 2 1 lists the flow cells available for use with the Dionex PDA STANDARD FLOW CELLS Cell Material Cell Cell Path Volume of Heat Intended Flow Volume Length Exchanger Rate Range Inlet Tubing PEEK 13 uL 10 mm 45 uL 0 5 to 5 0 mL min P N 056346 316 stainless steel 13 uL 10 m
123. the data collection rate is 20 Hz the 3D sample wavelength range must be lt 310 nm Example Chromatogram Selecting the Sample Wavelength Reference Wavelength and Reference Bandwidth Figure 3 8 shows the spectrum of caffeine The operating conditions are Sample wavelength 272 nm Bandwidth 5 nm Reference wavelength 325 nm Reference bandwidth 51 nm 50 Doc 065378 01 1 12 3 e Operation and Maintenance These settings calculate the absorbance by the following equation avg 300 to 350 AU 08 1 I 270 to 274 offset in AU at autozero at 272 nm Where Ix Light intensity Offset Absorbance offset at autozero 1 02 1200 AU 4 Bandwidth 5 nm 270 nm to 274 ni 7504 iW mAU 500 S i T 4 Reference Bandwidth 51 nm m H V i 300 to 350 nm d d NE 04 T 207 T T T E T T T T T am 220 238 250 263 1275 288 300 313 315 338 350 363 375 388 400 413 425 438 450 i nm Y Y 272 nm 325 nm Sample Wavelength Reference Wavelength Figure 3 8 Caffeine Spectrum Bunch Width The bunch width setting determines how many nanometers are averaged when collecting 3D data The default is 1 nm Selecting a bunch width above 1 nm will reduce the required data storage by approximately the reciprocal Do not select a bunch width when the spectrum of the compound has a fine structure the bunch width
124. ther module directly to the PC e Connect the detector to an external USB hub P N 060392 To connect the Dionex PDA directly to the PC 1 Plug the A connector of the USB cable P N 063246 into the USB port on the computer see Figure B 5 2 Plug the connector of the USB cable into a USB receptacle on the Dionex PDA rear panel USB Cable P N 063246 Plug the USB cable s B PC connector into the USB receptacle on the PDA Plug the USB cable s A connector into the USB port on the PC Figure B 5 Dionex PDA Connected Directly to the Chromeleon PC 120 Doc 065378 01 1 12 B Installation To connect the Dionex PDA to the internal USB hub of another module NOTE If you are installing a Dionex PDA with a Dionex ICS 5000 or Dionex ICS 3000 Ion Chromatography System refer to the system installation instructions for information about USB compatibility issues with these systems The manuals are available on the Thermo Scientific Reference Library DVD P N 053891 The USB standard limits the USB cable length to 5 meters 5 5 yds Each USB device can be separated from the PC by no more than five hubs Thus if five hubs are installed each USB device can be located no more than 30 meters 32 yds from the PC 1 Plug the A connector of the USB cable P N 063246 into the USB port on the module with the internal hub see Figure B 6 2 Plug the B connector of the U
125. time data collection rate Peak detection baseline noise linearity Set automatically by Chromeleon 6 8 not available in Chromeleon 7 Flow Cell Material The flow cell material must be chemically compatible with the mobile phases and analytes of interest Strong bases can etch the fused silica windows of the flow cell If the IMPORTANT mobile phase is a base make sure the mobile phase concentration does not exceed 0 1 M If the concentration of the base is greater than 50 mM disconnect the separator column and flush the system with deionized water for 5 minutes at 1 0 mL min immediately after the analysis If strong base remains in the cell for 1 to 2 days the cell windows may need to be replaced Do not use a PEEK flow cell with normal phase or chlorinated IMPORTANT solvents these solvents will damage the cell Doc 065378 01 1 12 43 Dionex PDA Operator s Manual Rise Time Do not use a stainless steel flow cell with low pH solutions these solutions may cause corrosion contamination and metal leaching Rise time is a measure of how quickly the Dionex PDA responds to a change in signal The selected rise time is applied to all data collected as well as to both analog and digital output The Dionex PDA rise time settings are 0 05 0 1 0 2 0 5 1 0 2 0 default or 5 0 seconds Select a rise time that is about 25 of the peak width at half height of the narrowest peak of interest A longe
126. ting 53 NOTES in this manual 8 O Operating parameters Optimization 43 53 Optical bench Cooling 21 68 Leak sensor 13 Leak tray 13 Location 13 Optical system Components 14 Illustration 14 P Panel tabset 27 Parts replacement 91 131 See also Service procedures Use of non Dionex parts 91 Passivation of stainless steel systems 56 PC boards Data Processing board 21 Index 4 Doc 065378 01 1 12 Index Preamp board 21 Repairs 20 PDA Control panel 36 129 Peak height 44 46 Peak identification 2 3 46 Peak purity 2 3 46 Peak purity analysis 30 Peak resolution 43 Peaks Asymmetrical 44 Co eluting 45 Correcting height problem 84 Identification 41 Improving shape 84 Resolution 43 PEEK flow cells 16 Chemical compatibility 17 25 43 113 See also Cells 16 PGM file 29 Photodiode array 2 14 15 Photodiode array detection Overview 2 Photodiode Array Detector 1 Automated control 41 Control panel 28 128 129 Dimensions 105 Direct control 38 Flow cells 2 15 Maintenance 55 Parts replacement 91 Performance optimization 43 53 Power cord 123 Power supply 20 105 Ship Kit 112 122 Shutdown procedure 55 Spare parts 131 Unpacking instructions 112 Warranty 91 Weight 105 Photodiode Array Panel ePanel 28 128 129 Post column reagents 84 Degassing 75 Power cord 23 103 123 POWER LED LED is lighted 12 Power requirements 1
127. tion Lamp Power Supply Board The lamp power supply controls the deuterium and tungsten lamps In addition it supplies power to the variable speed fan that cools the optical bench NOTE The fan speed is controlled automatically Changes in fan speed may be audible especially when the lamp selection is changed or the ambient temperature fluctuates SHOCK HAZARD Components used to ignite and operate the deuterium lamp are at high potentials WARNING et faire fonctionner la lampe au deut rium sont a des potentiels DANGER D ELECTROCUTION Les composants utilis s pour allumer VAN lev s AVERTISSEMENT STROMSCHLAGGEFAHR Die Komponenten zum Z nden und Betreiben der Deuteriumlampe f hren Hochspannung Der Service darf nur von qualifiziertem Personal durchgef hrt werden WARNUNG Preamp Board The photodiode array is connected directly to the preamplifier The preamp gain is automatically adjusted to compensate for system variables such as lamp intensity Analog to digital conversion of the signal occurs on the Preamp board Preamp output is directed to the Data Processing board Data Processing Board The Dionex PDA Moduleware resides on the Data Processing board This board provides the digital signal processing and conversion to log ratios when absorbance is measured Also located on the Data Processing board are the connectors for USB and TTL relay communications as well as four BNC connectors that provide th
128. tion and metal leaching A 5 3 Semi Preparative Flow Cell Cell Body Volume and Optical Path Length Maximum Operating Pressure Chemical Compatibility PEEK 0 7 uL volume 0 4 mm 0 02 in path length 10 34 MPa 1500 psi e Do not use bases stronger than 0 1 M these solutions will etch the fused silica windows of the flow cell e Do not use normal phase or chlorinated solvents with the flow cell these solutions will damage the cell A 6 Heat Exchangers Maximum Operating Pressure Volume of Standard Cell Heat Exchangers including cell inlet tubing PEEK cell 2 MPa 300 psi Stainless steel cell 3 MPa 500 psi PEEK cell 45 uL Stainless steel cell 20 uL 108 Doc 065378 01 1 12 A Specifications Volume of Semi PEEK cell 5 uL Micro Cell Heat Stainless steel cell 5 uL Exchangers including cell inlet tubing Doc 065378 01 1 12 109 Dionex PDA Operator s Manual 110 Doc 065378 01 1 12 B Installation B 1 Facilities Requirements e Make sure the installation site for the Thermo Scientific Dionex ICS Series Photodiode Array Detector Dionex PDA meets the power and environmental specifications listed in Appendix A e For mobile phase generation or when manually preparing mobile phase and regenerant use ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Table B 1 Contaminant Specification Ions Resistivity 218
129. turned on Turn on the lamp from Chromeleon or the TTL input When a lamp is on the corresponding LED DEUTERIUM UV or TUNGSTEN VIS is lighted Lamp LED flashing rapidly The corresponding lamp failed to power on properly Open the Chromeleon 7 Command window see page 31 or Chromeleon 6 8 Commands dialog box see page 32 and select UV Check that the required command UVLampPowerOnSetting or VisLampPowerOnSetting is On If the LED continues flashing replace the lamp See Section 5 7 or Section 5 8 for instructions on replacing the deuterium lamp or tungsten lamp respectively Detector and or ePanel not connected to instrument Chromeleon 7 detector and or Control panel not connected to timebase Chromeleon 6 8 For Chromeleon 7 In the Instrument Configuration program add the Dionex PDA device driver to an instrument For Chromeleon 6 8 In the Server Configuration program add the Dionex PDA device driver to a timebase Windows operating system does not recognize Dionex PDA When the computer is turned on Windows scans the network for unknown devices If the Dionex PDA power is off the detector cannot be identified If you connect the Dionex PDA to the PC before installing Chromeleon the detector cannot be identified See Section 4 14 for instructions on how to resolve this 74 Doc 065378 01 1 12 4 Troubleshooting 4 5 Noisy Baseline Mobile phase or post column reagent contains light absorbing
130. uration program or the Chromeleon 6 8 Server Configuration program see Section B 11 3 To open the Chromeleon 7 Command window 1 Open the ePanel Set for the instrument that includes the Dionex PDA 2 Click Command on the Instrument toolbar above the ePanel Set or press the F8 key The Command window appears see Figure 3 3 UV Aey Data_Collection Rate 10 00 j Gy UV Rely 2 DemoFileName 1 Uv TTL 1 DeviceType 175 3000 PDA Uv TTL 2 Fitmwateertion 110 EN UV Calbison Lamplintensity 390650 counts s UV Diagnostic ModuleAge 300 hour OC OP Negahreehbeorphorl evel 1 Gg System OpbcaBenchTeemperahure 26 C Qualfication GracePeriod 7d s gt Qualification Interval 180d Qualification LastDate 2010 04 26 Qualification Last perator Qualification W amingPenod 14d Rise Time 200 Figure 3 3 Command Window Doc 065378 01 1 12 39 Dionex PDA Operator s Manual 3 Click UV and then click the Properties tab or Commands tab to view detector properties or commands respectively To execute a command click the button next to the command NOTE change the display filter level right click the list of commands and select the desired filter on the context menu To open the Chromeleon 6 8 Commands dialog box 1 Open the Dionex PDA Control panel 2 Select Control gt Commands or press the F8 key The Commands dialog box appears see Figure 3 4 Commands PDA gg Uv ER 3DFIELD
131. velength Off Flowing water at 1 0 mL min 10 35 MPa 1500 psi 46 Doc 065378 01 1 12 3 e Operation and Maintenance 0 0400 WVL254 0 03004 WI h Bandwidth 8 Noise 14 uAU 0 02004 0 01004 0 zen P V NU Bandwidth 4 Noise 16 AU 0 01004 get 0 0300 1 if ui MW han IN N A n Wu H A ll Mu WI Ay i VII 1 Alix Au IN WEA Bandwidth 1 MIN MI Fifa jj N j J f I WA A d yn IV n m AL 1 1 Noise 26 AU 0 04004 WW Wu n N Ww N 20 0500 mir Figure 3 6 Effect of Bandwidth on Baseline Noise Reference Wavelength The reference wavelength is the center wavelength of the reference intensity determination Absorbance is measured by comparing the reference intensity to the sample intensity Selecting a reference wavelength implies a reference mode for each of the single wavelengths being collected There are two types of reference mode active or off e select the active reference mode enter a wavelength within the selected sample scanning range of the Dionex PDA The selected wavelength will be used as the reference wavelength The reference intensity will vary over time as the signal intensity changes For maximum compensation select a reference wavelength from the same lamp as the sample wavelength For example
132. wavelength is included in the wavelength range Wavelength range too narrow Make sure the spectrum wavelength range includes both the reference wavelength and reference bandwidth Make sure the peak absorbance wavelength is not included in the reference bandwidth Reference bandwidth too wide Select a narrower reference bandwidth The reference bandwidth should not overlap the bandwidth Doc 065378 01 1 12 83 Dionex PDA Operator s Manual 4 12 Peaks Too Large or Small Analog output related problem Check the recorder and integrator input voltage The Dionex PDA provides a 1 volt full scale output Verify that the selected output range AU full scale is appropriate System level problem Verify that the sample volume or concentration is appropriate Verify that the rise time see page 45 and data collection rate see page 46 are appropriate to capture the narrowest peak Prepare fresh post column reagent Verify that the reagent flow rate is correct Reference bandwidth too wide Select a narrower reference bandwidth The reference bandwidth should not overlap the sample bandwidth 4 13 Poor Peak Shape Concentration of standard is too high column is overloaded Dilute the standard Install a sample loop with a smaller volume Concentration of standard is too low Increase the standard concentration Inappropriate mobile phase Do not use a mobile phase that absorbs strongly at the peak absorbance wavelen
133. where little absorption occurs Thermo Fisher Scientific recommends selecting a reference wavelength below 380 nm for UV applications and above 600 nm for visible applications For more information see Reference Wavelength on page 47 Bandwidth is too narrow Select a wider bandwidth and reference bandwidth if appropriate for the application For guidelines when selecting the sample and reference bandwidths see Bandwidth on page 46 and Reference Bandwidth on page 50 76 Doc 065378 01 1 12 4 Troubleshooting e Front cover lamp cover or flow cell cover is missing Optical components are sensitive to temperature and light Do not operate the Dionex PDA unless the front cover lamp cover and flow cell cover are in place e Crimped or plugged tubing Over time tubing may become pinched off and plugged Periodically check all tubing and replace as needed see Section 5 1 Flow cell installed incorrectly Check that the cell is inserted straight into the optical bench and is fully seated e Inappropriate rise time In general the rise time should be approximately 2546 of the peak width at half height of the narrowest peak of interest See page 44 for more information Detector exposed to high vibration Optical detectors are sensitive to vibrations Make sure the Dionex PDA installation site is vibration free Filter paddle has malfunctioned If you have recently autozeroed the d
134. will reduce the spectral resolution Doc 065378 01 1 12 51 Dionex PDA Operator s Manual Step Chromeleon 6 8 only It is not necessary for the user to select a step setting the appropriate IMPORTANT rem step setting is selected automatically by Chromeleon 6 8 A Step is the time interval between two successively stored data points The smaller the step the more data points that are recorded and in general the more precise the analytical results However because collecting more data points requires more storage capacity the step setting sometimes represents a compromise between the amount of information collected and the file size Chromeleon 6 8 automatically selects the step value that is the inverse of the data collection rate selected by the user For example if the data collection rate is 5 0 Hz Chromeleon 6 8 sets the step to 0 2 second The following table indicates the step setting automatically selected for each data collection rate Data Collection Rate Hz 0 25 0 5 1 0 2 0 2 5 5 0 10 0 20 0 Step Override Step seconds 4 0 2 0 1 0 0 5 0 4 0 2 0 1 0 05 IMPORTANT This section explains how to override the step setting automatically selected by Chromeleon 6 8 This information is provided for reference for advanced users only Be aware that selecting an inappropriate step setting may cause loss of sensitivity skipped data points and other problems In almost all cases the st

ICS-Series Photodiode Array Detector Manual

Contents

Download Pdf Manuals

Related Search

Related Contents