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PDA-100 (USB)

1. 30 3 24 Direct Control te reme oa Nhs XA SEE CAES RES 30 3 22 Automated Control 33 Optimizing Detector Performance 4 Stand Alone Analog Operation 53 Routine Maintenance 54 4 Troubleshooting 4 1 4 2 4 3 4 4 4 5 4 6 4 7 4 8 4 9 4 10 4 11 4 12 4 13 4 14 Alarms and Error Conditions 57 Flashing 70 Lamp Does Not Light or Lamp LED Is Flashing 72 No Detector Response 72 Nisy Baselin Jn t ee ee Nee kee 73 Drifting Baseline eee ute eA ed eh 76 Deuterium Lamp Intensity Reading Too Low 77 Wavelength Calibration Fails 79 Wavelength Verification Fails 80 No Spectra Collected 81 Low Spectral Resolution 81 Peaks Too Large or Small 82 Poor Peak Shapes dee ose ha EHE 82 Faulty USB Communication 84 Doc 031898 03 3 06 Contents 4 15 Diagnostics eter res 84 4 15 1 Moduleware Run Time Diagnostics 84 4 15 2 Software Diagnostics and Calibration 85 5 Service gt 51 hiquid be
2. Figure 3 3 Effect of Rise Time on Baseline Noise 42 Doc 031898 03 3 06 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 PDA 100 The detector electronics collects data at up to 20 0 Hz The PDA 100 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 Slower data collection rates store the average of the 10 0 Hz points for example a 5 0 Hz rate stores the average of four 20 0 Hz points 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 e fall peaks are relatively wide select a slower data collection rate 1 0 Hz for example e If any peaks of interest are less than a few seconds select a faster data collection rate 5 0 Hz for example Ifthe 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 e 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
3. 108 B 3 2 Connecting the PDA 100 to the Chromeleon PC 109 B 3 3 Connecting the PDA 100 to an External USB Hub 109 B 3 4 Connecting the Power 110 B 3 5 Installing the Flow 112 B 3 6 Connecting the Waste Line 114 B 3 7 Making the Analog Output Connections 115 B 3 8 Making the Relay TTL Connections 115 C Reordering Information Doc 031898 03 3 06 1 Introduction 1 4 Product Overview The Dionex PDA 100 Photodiode Array Detector P N 064532 is an optical detector capable of measuring the absorbance spectrum from 190 to 800 nm 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 PDA 100 up to five single wavelengths 2D chromatograms can be collected without being required to collect 3D data Collecting individual wavelengths instead of the spectra offers two advantages it eliminates the need to perform extractions for analyses that do not require spectral data and it conserves disk space Key features of the PDA 100 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 filte
4. 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 In Chromeleon press F8 to display the Commands dialog box b Select UV and UV Calibration c Select Intensity and click Execute to calibrate the lamp intensity d Select Autozero in the Commands dialog box and click Execute 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 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 Dionex 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 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 b Ifthe error message appears again contact Dionex for assistance Filter paddle has malfunctioned Check the 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 65 for instructions
5. Parts replacement 87 117 See also Service procedures Use of non Dionex parts 87 Passivation of stainless steel systems 54 PC boards Data Processing board 19 Preamp board 19 Repairs 18 PDA 100 Photodiode Array Detector 1 Applications 29 Automated control 23 Dimensions 101 Direct control 23 30 32 Flow cells 1 13 Maintenance 54 Parts replacement 87 Performance optimization 41 49 51 Power cord 111 Power supply 18 101 Power switch 111 Safety standards 6 Ship Kits 107 Shutdown procedure 54 Spare parts 117 Unpacking instructions 107 Warranty 87 Weight 101 Peak height 42 44 Peak identification 2 3 44 Peak purity 1 3 44 Peak resolution 41 Peaks Asymmetrical 42 Co eluting 43 Correcting height problem 82 Improving shape 82 Resolution 41 PEEK flow cells 14 Chemical compatibility 15 25 41 112 See also Cells 14 PGM files 23 33 81 Creating a program automatically 33 Creating a program manually 33 PGM Wizard 23 33 Photodiode array 1 12 13 Photodiode array detection Overview 2 Index 4 Doc 031898 03 3 06 Index Post column reagents 82 Degassing 74 Power cord 20 99 111 Power LED 10 Flashing 10 80 Power requirements 101 Power supply 18 Power switch 111 Power up diagnostic tests 10 Preamp board 19 Preamp gain 19 Problems See Troubleshooting Pumping system requirements 26 R Rear panel Analog output connectors 22
6. 5 00 s Start settings and data acquisition times Be cet es ncm etra nee RefWavel nm 1 pv VIS 1 0 000 30 000 210 0 2 uv vis 2 0 000 30 000 254 0 3 vis 3 0 000 30 000 272 10 0 4 Uv vis 4 0 000 30 000 520 10 0 5 zuv vis 5 0 000 30 000 600 10 0 v 3DFIELD 750 D 3D Min Wavelength 200 190 790 nm 3D Bunchwidth 2 1 25 nm 3D Wavelength 800 200 800 nm en 8 Enter Data Collection Rate and the Rise Time NOTE When the data collection rate is set to 10 0 Hz the 0 05 second rise time setting is not available When the data collection rate is set to 20 0 Hz the 5 0 second rise time setting is not available NOTE The 20 0 Hz data collection rate and 0 05 second rise time settings are not supported unless PDA 100 Moduleware version 1 1 0 or later is installed 9 To program UV_VIS_1 through UV VIS 5 the single wavelength channels a Check or clear a check box to determine whether 2D data from this channel will be collected b Foreach selected channel enter the starting and ending data acquisition times as well as the wavelength bandwidth reference wavelength and reference bandwidth 36 Doc 031898 03 3 06 3 Operation and Maintenance NOTE The settings for these channels apply to both analog outputs and digital outputs UV channel 1 analog output 1 UV2 analog output 2 et
7. DIONEX PDA 100 USB PHOTODIODE ARRAY DETECTOR OPERATOR S MANUAL Now sold under the Thermo Scientific brand Thermo SCIENTIFIC Document No 031898 Revision 03 March 2006 2006 by Dionex Corporation All rights reserved worldwide Printed in the United States of America This publication is protected by federal copyright law No part of this publication may be copied or distributed transmitted transcribed stored in a retrieval system or transmitted into any human or computer language in any form or by any means electronic mechanical magnetic manual or otherwise or disclosed to third parties without the express written permission of Dionex Corporation 1228 Titan Way Sunnyvale California 94088 3603 U S A DISCLAIMER OF WARRANTY AND LIMITED WARRANTY THIS PUBLICATION IS PROVIDED AS IS WITHOUT WARRANTY OF ANY KIND DIONEX CORPORATION DOES NOT WARRANT GUARANTEE OR MAKE ANY EXPRESS OR IMPLIED REPRESENTATIONS REGARDING THE USE OR THE RESULTS OF THE USE OF THIS PUBLICATION IN TERMS OF CORRECTNESS ACCURACY RELIABILITY CURRENTNESS OR OTHERWISE FURTHER DIONEX CORPORATION RESERVES THE RIGHT TO REVISE THIS PUBLICATION AND TO MAKE CHANGES FROM TIME TO TIME IN THE CONTENT HEREINOF WITHOUT OBLIGATION OF DIONEX CORPORATION TO NOTIFY ANY PERSON OR ORGANIZATION OF SUCH REVISION OR CHANGES TRADEMARKS BioLC Chromeleon and SUMMIT are trademarks or registered trademarks of Dionex Corporation Teflon
8. WARNING The power supply cord is used as the main disconnect device Make sure the socket outlet is located near the PDA 100 and is easily accessible CAUTION Operation at AC input levels outside of the specified operating voltage range may damage the PDA 100 CAUTION 20 Doc 031898 03 3 06 2 Description 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 la AVERTISSEMENT terre Le cordon d alimentation principal est utilis comme dispositif N principal de d branchement Veillez ce que la prise de base soit situ e install e pr s du module et facilement accessible 1 DANGER D LECTROCUTION Pour viter toute lectrocution il faut MISE EN GARDE STROMSCHLAGGEFAHR Zur Vermeidung von elektrischen Schl gen ist eine geerdete Steckdose zu verwenden Das Ger t darf nicht ohne Erdung betrieben bzw an Wechselstrom angeschlossen WARNUNG werden Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung AN Stellen Sie sicher daB sich die Steckdose nahe am Ger t befindet und leicht zug nglich ist VORSICHT Fuses The fuse holder is part of the main power receptacle The PDA 100 uses two 4 0 amp fast blow IEC 127 fuses P N 954763 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 specifi
9. 031898 03 3 06 51 PDA 100 USB Photodiode Array Detector In Chromeleon press F8 to display the Commands dialog box Select UV and then select NegativeAbsorptionLevel Enter a new setting and click Execute Select Autozero in the Commands dialog box and click Execute to run the autozero routine Select LampIntensity in the Commands dialog box 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 UV Calibration Intensity and click Execute 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 52 Doc 031898 03 3 06 3 Operation and Maintenance 3 4 Stand Alone Analog Operation Section 3 4 describes limited stand alone operation of the PDA 100 when the detector is not interfaced to a computer running Chromeleon In stand alone operation TTL inputs on the PDA 100 rear panel can be used to trigger autozero or to turn the lamps on and off All other detector parameters will remain at their factory default settings and canno
10. If RefWavelength is Off the reference value is the first data point of the sample wavelength and bandwidth after autozero is performed Doc 031898 03 3 06 23 PDA 100 USB Photodiode Array Detector PDA 100 Command Rise_Time Step TTL_Input_ Mode UV_Lamp UVLampAge UVLampPowerOnSetting Visible Lamp VisLampAge VisLampPowerOnSetting Wavelength WavelengthCal WavelengthCalResult WavelengthVerTest WavelengthVerTestResult Function Sets how quickly the detector responds to a change in signal Sets the step which is the time interval between two successively stored data points Sets the TTL input signal mode Turns the deuterium lamp on and off Reports or resets the number of hours the deuterium lamp has been on Selects the power up setting for the deuterium lamp 1 whether the lamp is turned on whenever the detector is turned on The default setting is On Turns the tungsten lamp on and off Reports or resets the number of hours the tungsten lamp has been on Selects the power up setting for the tungsten lamp 1 e whether the lamp is turned on whenever the detector is turned on The default setting is On Sets the sample wavelength up to five sample wavelengths can be programmed Runs the wavelength calibration procedure to improve wavelength accuracy in the UV range The result of the last wavelength calibration procedure Performs the wavelength verification test
11. PDA 100 USB Photodiode Array Detector 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 Dionex for assistance NOTE The PDA 100 electronics cannot be serviced by users All repairs of the electronics components must be performed by Dionex 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 4 2 Flashing LED Run LED is flashing 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 70 Doc 031898 03 3 06 4 Troubleshooting e Deuterium LED is flashing The lamp did not power on properly Check the Chromeleon Audit Trail for a lamp related error message If necessary replace the lamp see Section 5 7 If the LED flashes again there may be a bad connection between the lamp power supply and the lamp Contact Dionex for assistance NOTE The PDA 100 electronics cannot be serviced by users All repairs of the electronics components must be pe
12. and Tefzel are registered trademarks of E I duPont de Nemours amp Company PRINTING HISTORY Revision 01 April 2004 Revision 02 July 2004 Revision 03 March 2006 Contents 1 Introduction 1 1 1 2 1 3 1 4 Product Overview cs sues dda ele ean dew or HR fora ala ft EE 1 Theory of Photodiode Array Detection 2 1 2 1 Advantages of Photodiode Array Detection 2 Overview of This Manual 5 Safety and Regulatory Information 6 1 4 1 Safety Messages 6 1 4 2 Product Labels EE EEN o e us 7 2 Description 2 1 Front Panel 9 22 Inside Front Panel se ecd stas adh hed eme aaa anes 11 23 Optical Systems espese eR feci ed 12 2 3 1 FHowCelsiii n le A ay RR Pea See 14 2 4 Electronics os RR RR REG OE ae ha dae eee ee ba 18 2 5 RearPanel ces ween nes RR E ROSES Ee 20 2 6 Chromeleon Software 23 2 7 Mobile Phases ccce eau ccd ed a ed ee ede ee 25 2 8 Solvent Delivery 26 Doc 031898 03 3 06 i PDA 100 USB Photodiode Array Detector 3 Operation and Maintenance 3 1 3 2 3 3 3 4 3 5 Getting Started oru EDI ee Make Re ats 29 Routine
13. and flow cell cover are in place B 2 Unpacking the PDA 100 e Carefully remove the PDA 100 from the shipping container Lift the PDA 100 by the side or bottom only the front panel of the IMPORTANT Sei detector snaps into place and must not be used for lifting e Do not turn on the PDA 100 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 mains power e Unpack all items in the PDA 100 Ship Kit P N 060977 and check them against the packing list If there are any discrepancies notify Dionex immediately Doc 031898 03 3 06 107 PDA 100 USB Photodiode Array Detector Installation B 3 1 Note on ICS 3000 System Installations If you are installing a PDA 100 with an ICS 3000 Ion Chromatography System refer to CS 3000 Ion Chromatography System Installation Instructions Document No 065032 The manual contains specialized information including details about USB compatibility issues with ICS 3000 systems Before You Begin Before going on to Section B 3 2 or Section B 3 3 verify that the following tasks have been completed e Chromeleon software is installed on the computer The Chromeleon license is installed If you are not sure how to install the software and or license refer to Installing the Chromeleon Chromatography Management System
14. 4 WARNING CAUTION Figure B 2 Three USB Devices Connected to a USB Hub Connecting the Power Cord SHOCK HAZARD To avoid electrical shock use a grounded receptacle Do not operate the PDA 100 or connect it to AC power mains without an earthed ground connection The power supply cord is used as the main disconnect device Make sure the socket outlet is located near the PDA 100 and is easily accessible 110 Doc 031898 03 3 06 B Installation Operation at AC input levels outside of the specified operating voltage range may damage the PDA 100 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 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 Gerat darf nicht ohne Erdung betrieben bzw an Wechselstrom angeschlossen WARNUNG werden gt Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung Stellen Sie sicher da sich die Steckdose nahe am Ger t befindet und leicht zuganglich ist gt VORSICHT Connect a m
15. 79 Intensity 55 Lamp does not light 72 Maintenance 55 On off control 24 Output waning 75 Part number 117 Power supply 19 Power up setting 24 Replacing 94 Resetting the lamp age 85 See also Lamps Time in use 96 98 Time to stabilize 29 74 77 Deuterium LED 10 Flashing 10 72 73 Diagnostic procedures 57 Chromeleon 85 PDA 100 Moduleware 84 Dionex Technical Support 29 57 87 Disk space 41 43 44 Conserving 1 44 Drain tube 22 114 E Electrical specifications 101 Electromagnetic interference EMI 18 Electronics 18 Repair 87 Electrostatic discharge ESD 18 Equilibration system 74 Error messages 9 11 Index 2 Doc 031898 03 3 06 Index F Fan 19 67 Speed 19 Ferrule fittings 66 73 88 Part number 114 Filter paddle 12 13 Malfunction 76 78 Positions 13 Flow cells See Cells See Type of cell Front panel Illustration 9 LEDs described 10 11 Fuses 21 101 Part number 117 Replacing 99 G Gradient applications 26 51 Reference wavelength selection 46 77 Grating optical 12 13 H Heat exchangers 15 17 104 Operating pressure 104 Tubing connections 88 Volume 14 104 105 Holmium oxide filter 1 13 Filter paddle positions 13 Wavelength verification 13 Hub USB 109 Humidity operating 101 I ICS 3000 Ion Chromatography System 108 Installation instructions 108 Important icon 6 Inside front panel 1
16. A PDA detector can collect spectra of each peak after which the PDA software can calculate the absorbance maximum Detection of multiple wavelengths A PDA 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 PDA 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 PDA detector is used spectra are automatically collected as each peak elutes The PDA 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 1 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 these peaks might have been misidentified as the same component A PDA 100 under the control of Chromeleon with the 3D Data Acquisition license correctly identified and differentiated the components The spectra o
17. AUTOSAMPLER PAN the 3D panel monitors chromatograms contour plots and spectra online see Figure 3 2 NOTE The 3D Control panel is not available unless Chromeleon includes the 3D Data Acquisition license Open a Control panel by double clicking its name in the list 30 Doc 031898 03 3 06 3 Operation and Maintenance Acquisition On Off 510 000 UV VIS 3AcqOn 000 UV_VIS_4 AcqOn 000 UV VIS 5 AcqOn 21 308 StopFlow Serial Numbers om d 3d m au a sz 3 zm E Figure 3 1 PDA 100 2D Control Panel Example 5 The Control panel is initially unconnected to the PDA 100 timebase To connect the panel to the timebase open the Control menu and click the name of the timebase from the list at the bottom of the menu 6 Select the operating parameters 7 Turn on the pump Set the flow rate and mobile phase composition 8 Click the Acquisition On Off toolbar button to begin manual data acquisition Doc 031898 03 3 06 31 PDA 100 USB Photodiode Array Detector Serial Numbers Acquisition On Off Chromeleon Autosampler Pump PDA 3D Timebase PDA1 TEST Computer name PDA Fie Edt View Workspace Qualification Control Batch Window laj o s elles ODER EET EET FE DEERE Sample Audit Trail Datasource PDA1 local ElapsedTime 0 674 13 48 20 0 000 Sampler Wailing far inject response on AS OOinjectState 2 Seq
18. Failure of an electronics component Turn off the PDA 100 power and contact Dionex for assistance NOTE Do not attempt to service the PDA 100 electronics components All repairs of the electronics components must be performed by Dionex personnel 78 Doc 031898 03 3 06 4 Troubleshooting 4 8 Wavelength Calibration Fails e Deuterium lamp may be defective If the Deuterium LED is flashing or if the LED fails to light replace the deuterium lamp see Section 5 6 If the Deuterium LED is lighted but is not flashing open the PDA 100 Wellness panel and run the wavelength calibration and the wavelength verification test see Section 4 15 2 If the PDA 100 fails these procedures remove the flow cell from the detector and repeat both procedures If the detector fails the wavelength calibration again contact Dionex for assistance e Deuterium lamp intensity out of calibration 1 Remove the cell from the optical bench see Section 5 4 2 Check the deuterium lamp intensity a b In Chromeleon press F8 to display the Commands dialog box 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 b In Chromeleon press F8 to display the Commands dialog box Select UV and UV_Calibration Select Intensity and click Execute to calibrate the lamp inte
19. continuous flow at 0 2 mL min This rinses corrosive acids salts or bases from the flow paths 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 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 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 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
20. control you create a PGM file or program which is a list of time precise control commands for automated operation of the PDA 100 PGM files can be created automatically with the help of a software wizard or manually by editing an existing PGM file Chromeleon includes many control commands that are available for all detectors Several additional commands are available exclusively for the PDA 100 see the table below You can select these commands from either the default Control panel or the Commands dialog box To open the Commands dialog box press F8 or select Command on the Control menu PDA 100 Command Bandwidth BunchWidth Data Collection Rate NegativeAbsorptionLevel Offset Level RefBandwidth RefWavelength Function Sets the bandwidth the wavelength range at which the chromatogram is measured of the sample wavelength Determines how many nanometers are averaged when collecting 3D data Bunching or averaging the signals of adjacent wavelengths reduces the size of the 3D data stored Sets the rate at which Chromeleon collects digital data points from the detector Adjusts the negative absorbance this permits the baseline and peaks to be seen even when the mobile phase decreases absorbance Sets the offset applied to the recorder output Sets the bandwidth of the reference wavelength if one is selected If RefWavelength is Off the RefBandwidth setting has no effect Sets the reference wavelength
21. corresponding front panel LED Deuterium or Tungsten is lighted Lamp LED flashing The corresponding lamp failed to power on properly In Chromeleon press F8 to display the Commands dialog box and select UV Check that the 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 Control panel not connected to timebase In the Chromeleon Server Configuration program add the PDA 100 device driver to a timebase For details refer to the Chromeleon Help or user s guide Windows operating system does not recognize PDA 100 When the computer is turned on Windows scans the network for unknown devices If the PDA 100 power is off the detector cannot be identified If you connect the PDA 100 to the computer before installing Chromeleon a Windows message box requesting a USB configuration file cmwdmusb inf will appear when you turn on the computer See Section 4 14 for instructions on how to resolve this Noisy Baseline Mobile phase or post column reagent contains light absorbing impurities Prepare all mobile phases and reagents with spectro grade solvents reagent grade chemicals and ASTM Type I or better filtered deionized water Leaking fittings Locate the source of the leak Tighten or replace all liquid line connections If the connectio
22. 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 82 Doc 031898 03 3 06 4 Troubleshooting e Inappropriate mobile phase Do not use a mobile phase that absorbs strongly at the peak absorbance wavelength e 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 44 Incorrect reference wavelength selected Select a different reference wavelength For guidelines to follow when selecting the reference wavelength see page 45 e 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 e 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 absor
23. 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 54 Doc 031898 03 3 06 3 Operation and Maintenance e 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 replace the lamp To check the lamp lifetime 1 In Chromeleon press F8 to display the Commands dialog box and select UV 2 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 e Check the deuterium lamp intensity approximately every 6 months 1 In Chromeleon press F8 to display the Commands dialog box and select UV 2 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 Commands dialog box select UV Calibration select Intensity and click Execute 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 verificatio
24. it is not necessary for users to select a step setting A step 1s 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 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 the software sets the step to 0 2 second The following table indicates the step setting automatically selected for each data collection rate Doc 031898 03 3 06 49 PDA 100 USB Photodiode Array Detector IMPORTANT Data Collection Rate Step Hz seconds 0 25 4 0 0 5 2 0 1 0 1 0 2 0 0 5 2 5 0 4 5 0 0 2 10 0 0 1 20 0 0 05 Step Override This section explains how to override the step setting automatically selected by Chromeleon 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 step setting selected by Chromeleon is the preferred setting However it is possible to override this setting by manually changing the step in the PGM file or on the Contr
25. on the emission spectrum from the deuterium lamp 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 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 In the Browser navigate to the following folder Dionex Templates Panels Dionex ICPDA 100 USB Wellness Open the PDA 100 Wellness panel Doc 031898 03 3 06 85 PDA 100 USB Photodiode Array Detector d Click the wavelength script button under Calibration The detector will perform the wavelength calibration routine and upload the result pass or fail to Chromeleon Wavelength verification Purpose Tests the accuracy of the selected wavelength The result of the last wavelength verification test is stored in the calibration log and can be retrieved at any time a Inthe Browser navigate to the following folder Dionex Templates Panels Dionex_IC PDA 100 USB Wellness b Open the PDA 100 Wellness panel c Click the wavelength verification script button under Diagnostics The detector will perform the wavelength verification test and upload the result pass or fail to Chromeleon 86 Doc 031898 03 3 06 5 e Service This chapter describes routine PDA 100 service procedures that users may perform All procedures not described here must be performed by Dionex p
26. 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 PDA 100 reports There are two ways to review this information e Check the Audit Trail displayed in the PDA 100 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 84 Doc 031898 03 3 06 4 Troubleshooting 4 15 2 Software Diagnostics and Calibration Chromeleon includes comprehensive diagnostics for the PDA 100 This section describes some of the most frequently used diagnostic procedures For more information refer to the Chromeleon Help or user s guide 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 press F8 to display the Commands dialog box Select UV Select the UVLampAge command for the deuterium lamp or VisLampAge command for the tungsten lamp Reset the number to zero Click Execute NOTE When the detector 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 Wavelength calibration Purpose Improves wavelength accuracy in the UV range by reassigning new wavelengths to each pixel based
27. the application For guidelines when selecting the sample and reference bandwidths see page 44 and page 45 Front panel lamp cover or flow cell cover is missing Optical components are sensitive to temperature and light Do not operate the PDA 100 unless the front panel 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 e 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 25 of the peak width at half height of the narrowest peak of interest See page 42 for more information Doc 031898 03 3 06 75 PDA 100 USB Photodiode Array Detector 4 6 Detector exposed to high vibration Optical detectors are sensitive to vibrations Make sure the PDA 100 installation site is vibration free Filter paddle has malfunctioned If you have recently autozeroed the detector check the 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 65 for instructions 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 R
28. the PDA 100 Control panel Detector and PGM file or Control panel connected to different timebases In Chromeleon add the detector to the same timebase as the PGM file or the PDA 100 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 wavelength is included in the wavelength range Doc 031898 03 3 06 81 PDA 100 USB Photodiode Array Detector 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 4 12 Peaks Too Large or Small Analog output related problem Check the recorder and integrator input voltage The PDA 100 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 42 and data collection rate see page 43 are appropriate to capture the narrowest peak Prepare
29. the Sample Wavelength Reference Wavelength and Reference Bandwidth Figure 3 6 shows the spectrum of caffeine The operating conditions are Sample wavelength 272 nm Bandwidth 5 nm Reference wavelength 325 nm Reference bandwidth 51 nm These settings calculate the absorbance by the following equation avg 2 300 to 350 AU log 5 U 108 See 270 to 274 offset in AU at autozero at 272 nm Where Ix Light intensity Offset Absorbance offset at autozero 48 Doc 031898 03 3 06 3 Operation and Maintenance 1200 WA Bandwidth 5 nm Wi DE 270 nm to 274 nm CN 750 7 i is dB mAU ai i n A 4 Reference Bandwidth 51 nm 5 Qo pm qao to 350 nm 20 T i T T T T T T T T T 220 238 250 263 1275 288 300 313 385 338 350 363 375 388 400 413 425 438 450 i nm Y Y 272 nm 325 nm Sample Wavelength Reference Wavelength Figure 3 6 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 will reduce the spectral resolution Step Chromeleon automatically selects the appropriate step setting IMPORTANT AT Therefore
30. 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 44 Doc 031898 03 3 06 3 Operation and Maintenance EEr Example Chromatogram Selecting the Bandwidth Figure 3 4 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 wavelength Off Flowing water at 1 0 mL min 10 35 MPa 1500 psi 0 02004 0000 0 01004 0 0200 0 03004 0 04004 3 0040037 ooo 0 01004 Bandwidth 8 W Noise 14 LAU Bandwidth 4 Noise 16 LAU Li d SAL h Mh MI UI I IA Mn M a hl M MIU dii di AJ Di M d d Bandwidth 1 HU i IV WUL Noise 26 pau i
31. the tubing guide in the lamp cover see Figure 5 1 6 Squeeze the handle of the flow cell and pull it out of the optical bench AL 9 ml Cell Inlet Tube Figure 5 1 Removing the Flow Cell from the Optical Bench Flow cell cover not shown 90 Doc 031898 03 3 06 5 Service 5 5 Replacing the Flow Cell Windows Contaminated 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 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 PDA 100 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 too
32. time of 0 5 second results in a system response longer than 2 0 seconds e Ata 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 The table below lists 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 Doc 031898 03 3 06 43 PDA 100 USB Photodiode Array Detector Rise Time Data Collection Rate seconds Hz 1 0 2 0 2 0 1 0 5 0 0 5 Sample Wavelength The PDA 100 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 PDA 100 can run five separate wavelengths without being required to collect 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
33. 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 deutertum 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 Dionex offers five cells for use with the PDA 100 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 Open Light passes unobstructed along the light path when the holmium oxide filter is moved out of the light path Blocked No light passes along the light path used to measure the dark signal without turning off the lamps 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 measure
34. 0 can be optimized by careful selection of key operating parameters Section 3 3 defines these parameters describes how they interact and offers guidelines for selecting them This table summarizes the topics discussed here 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 time data collection rate Peak detection baseline noise linearity Set automatically by Chromeleon 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 b
35. 1 Access to panel 11 Illustration 11 Installation Chromeleon software 108 Instructions 114 116 PDA 100 with ICS 3000 system 108 Site requirements 101 107 Integrator Analog output connections 115 Input voltage 82 Isocratic applications Reference wavelength selection 46 77 L Lamp intensity 55 Lamp power supply board 19 Lamps 1 Calibration 79 Deuterium LED flashing 10 Failure 10 Installation procedures 94 97 See also Deuterium lamp See also Tungsten lamp Tungsten LED flashing 10 Leak sensor 11 Leak tray 11 Maintenance 22 54 Leaks Prevention 22 Symptoms 54 LEDs on front panel 10 Lenses 13 Liquid leaks 88 Liquid lines Maintenance 54 Lithium battery disposal 87 Doc 031898 03 3 06 Index 3 PDA 100 USB Photodiode Array Detector M Maintenance procedures 54 Mise en garde icon 6 Mobile phases 26 Concentration guidelines 14 25 41 Degassing 25 74 Effect of pH on retention time 25 Lamp stability after changing 74 77 Preparation 73 Reservoir material 26 Solvent quality 25 Temperature stabilization 15 16 Moduleware 19 36 Diagnostic procedures 57 84 N Negative absorbance 23 41 76 Definition 51 Guidelines for selecting 51 NOTES in this manual 7 O Offset level 23 Operating parameters Optimization 41 49 51 Optical bench Cooling 19 67 Leak sensor 11 Leak tray 11 Location 11 Optical system Components 12 Illustration 12 P
36. 3 Windows replacement kit 91 Windows replacement procedure 91 92 Step 24 41 Definition 49 Guidelines for selecting 49 Selection by software 49 66 System equilibration 74 T Technical Support 29 57 87 Temperature ambient 101 Reference mode selection 46 Timebase connections 73 81 Troubleshooting Baseline drift 76 77 Baseline noise 73 76 Elution time is slow 74 Lamp does not light 72 PDA 100 does not respond 72 73 Peak shape is poor 82 Peak size is too big or small 82 Spectra not collected 81 Spectral resolution is poor 81 USB communication problem 84 Wavelength calibration fails 79 Wavelength verification fails 80 TTL control 22 115 Input mode 24 Installation 115 Pin assignments 116 Tubing connections 26 Maintenance 54 Tungsten lamp 12 13 Age command 24 Index 6 Doc 031898 03 3 06 Index Calibration 79 Lamp does not light 72 On off control 24 Output waning 75 Part number 117 Power supply 19 Power up setting 24 Replacing 97 Resetting the lamp age 85 See also Lamps Time in use 98 Time to stabilize 29 74 77 Tungsten LED 10 Flashing 10 72 73 Twisted wire assembly Part number 117 U USB 1 102 Communication problem 84 Configuration file 73 84 Connection to hub 109 Connector on rear panel 22 USB cable Installation 109 110 Part number 117 USB driver 108 UV wavelengths 13 V Verification w
37. 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 14 Doc 031898 03 3 06 2 Description IMPORTANT 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 leaching Standard Flow Cell The standard flow cell assembly see Figure 2 4 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 Ee Cell Outlet Tubing Reducing Union Fitting p Reducing Union Fitting Cell Inlet Tubing mA HY Heat Exchangers Pa KJ Spring Clip Figure 2 4 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 055
38. 61 060498 064169 057304 055903 043276 043275 060498 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 4 9 meters 16 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 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 PDA 100 flow cell windows replacement kit Semi Micro Flow Cell PEEK PEEK semi micro flow cell with heat exchangers PEEK semi micro flow cell outlet tubing assembly Reducing union fitting PEEK Ferrule Nut PDA 100 flow cell windows replacement kit Doc 031898 03 3 06 117 PDA 100 USB Photodiode Array Detector Part Number Item 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 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 asse
39. 7 fuses P N 954763 Dionex recommends always replacing both fuses 5 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 6 Reconnect the power cord and turn on the power 100 Doc 031898 03 3 06 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 4 0 amp fast blow IEC 127 fuses P N 954763 A 2 Physical Dimensions Height 17 5 cm 6 9 in Width 38 6 cm 15 2 in Depth 49 0 cm 19 3 in Clearance required behind detector 6 cm 2 4 in Weight 16 kg 35 lbs Decibel Level lt 50 dbA during routine operation 56 dbA at power up A 3 Environmental Operating 4 to 40 C 40 to 104 F constant temperature Temperature Operating 5 to 95 relative humidity noncondensing Humidity Doc 031898 03 3 06 101 PDA 100 USB Photodiode Array Detector A 4 Detector Optical System Light Sources 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
40. 903 P N 055902 Doc 031898 03 3 06 15 PDA 100 USB Photodiode Array Detector Semi Micro Flow Cell The semi micro 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 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 Cell Outlet Tubing Reducing Union Fitting IR a Cell Inlet Tubing N ff pIE Flow Cell Reducing Union Fitting 7 Heat Exchangers i KA Spring Clip Figure 2 5 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 Doc 031898 03 3 06 2 Description Semi Preparative Flow Cell The semi preparative flow cell assembly see Figure 2 6 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 Union Fitting c 0 51 mm 0 020 in I
41. Clearance required 76 Fuses 21 Illustration 20 111 Power cord connection 20 Relay TTL connectors 22 USB connector 22 Waste line 22 Recorder Analog output connections 115 Input voltage 82 Reference bandwidth 23 41 Definition 48 Guidelines for selecting 45 46 48 Reference intensity 45 Reference modes 45 Active reference 45 46 76 See also Reference wavelength Turning off active reference 46 Reference wavelength 23 41 45 46 48 76 Definition 45 Effect on baseline drift 47 Guidelines for selecting 45 46 Inappropriate setting 75 Relay control 22 115 Installation 115 Pin assignments 116 Relay TTL connector 22 115 116 Part number 117 Replacing parts 87 Use of non Dionex parts 87 Retention time 25 Rise time 24 41 Correlation with data collection rate 43 Definition 42 Effect on baseline noise 42 Guidelines for selecting 42 43 Inappropriate setting 75 Run LED 10 Flashing 11 S Safety icons in this manual 6 7 Safety messages in this manual 6 Sample bandwidth Guidelines for selecting 45 Sample intensity 45 Sample rate See Data collection rate Sample wavelength 24 Guidelines for selecting 44 Semi micro flow cells 13 Chemical compatibility 104 Flow rate range 14 Heat exchanger volume 14 Operating pressure 103 Optical path length 14 103 Overview 14 Replacement procedure 93 See also Cells Volume 14 103 Windows replacement kit 91 Windo
42. 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 t 10 LAU at 254 nm 2 second rise time 4 nm bandwidth and flowing water at 1 0 mL min t 15 at 520 nm 2 second rise time 10 nm bandwidth and flowing water at 1 0 mL min lt 15 n AU at 254 nm 2 second rise time 4 nm bandwidth and flowing water at 1 0 mL min lt lt 15 n AU 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 software the Chromeleon PC and the detector are connected through USB Universal Serial Bus 102 Doc 031898 03 3 06 A Specifications 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
43. D PIN 042627 P N 042855 Handle E N Union Fitting ZZ Ch NOE SS a Spring Clip Cell Inlet Tubing i 2 Flow Cell 0 51 mm 0 020 in ID PIN 042855 Figure 2 6 Semi Preparative Flow Cell Assembly Doc 031898 03 3 06 17 PDA 100 USB Photodiode Array Detector 2 4 Electronics Do not attempt to access the PDA 100 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 appropriate CAUTION electrostatic 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 PDA 100 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 mains and provides regulated low voltage power for the PDA 100 Power entry components are shielded and filtered to prevent electromagnetic interference EMI SHOCK AND FIRE HAZARD The po
44. F8 to display the Commands dialog box 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 Dionex for assistance NOTE The PDA 100 electronics cannot be serviced by users All repairs of the electronics components must be performed by Dionex personnel Invalid rise time Valid rise times at 20 Hz 0 05 0 1 0 2 0 5 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 Doc 031898 03 3 06 65 PDA 100 USB Photodiode Array Detector Invalid step for the 3DFIELD Valid steps 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 automatically selects the step value that is the inverse of the data collection rate see Step on page 49 In future accept the value selected by the software Only advanced users should override the step setting selected by IMPORTANT 3 Chromeleon Selecting an inappropriate step setting may cause loss of sensitivity skipped data points and other prob
45. I NN WW A A Wl I IN d Wi UN INI II d di i n IN d 20 0500 Figure 3 4 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 To select the active reference mode enter a wavelength within the selected sample scanning range of the PDA 100 The selected wavelength will be used Doc 031898 03 3 06 45 PDA 100 USB Photodiode Array Detector 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 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 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 The active reference mode minimizes baseline drift and is ideal for gradient analyses where t
46. L Time Device State Duration EHI Pump_TTL_2 230 Pump_Relay_1 Closed 138 00 ER UV Relay 1 0 00 Pump Injectvalve InjectPosition 30 00 H UV Relay 2 a g Uv TTL 1 E Uv TTL 2 gt Indicates or sets the device s state r Help 14 15 NOTE If you have already selected these parameters on the device page for a particular module the list box on the Relay and State Devices Options page already contains this information If you change any settings here Chromeleon will automatically copy the changes to the appropriate device page Select a device in the tree control Optional Enter the Retention Time for the selected device If you do not enter a time the entry appears in the initialization section of the PGM file 38 Doc 031898 03 3 06 3 Operation and Maintenance 16 Specify the State or Duration Clicking State in the tree control specifies a simple switch command Select Open or Closed from the drop down list box Clicking a state description in the tree control sets the device to the selected state and lets you specify a Duration Enter the duration of the selected state in the edit box 17 To add the following information to the list box click Add e Retention Time value e Name of the selected Device e State or Duration value Chromeleon will automatically organize all entries in the list box in chronological order To remove an entry from the list bo
47. acceptable for a PEEK system Other solvents and high concentrations of acetonitrile require a stainless steel system All tubing connections should be Teflon 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 s manual To avoid contamination always wear latex gloves that are lint free IMPORTANT i e 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 To clean the pump and system between applications 1 2 Remove the column and the suppressor if installed Connect the line exiting the injection valve directly to the flow cell inlet tubing Flush the system with deionized water at 1 0 mL min for 20 minutes 26 Doc 031898 03 3 06 2 Description 4 Flush the system with methanol at 1 0 mL min for 20 minutes For very sensitive applicat
48. aks noresi ss carte at eet 88 52 Cleaning the Flow Cell ars ed eee eh 89 5 3 Removing Trapped Air from the Flow Cell 89 5 4 Removing the Flow Cell from the Optical Bench 90 5 5 Replacing the Flow Cell Windows 91 5 6 Replacing the Flow Cell 93 5 7 Replacing the Deuterium 94 5 8 Replacing the Tungsten 97 5 9 Replacing the Main Power Fuses 99 A Specifications gol aS ord CA ERO DAD EE EN 101 2 Physical nee eu P ve T He RR EI Kee dete A A 101 AB BhnyItonmental OI ente hone b qe UR o ben qnae dts aca Aene 101 AA detector EEN 102 Ac Flow Gels ie l i une e De RU e PE Rer cen Mes yop ua 103 A 5 1 Standard Flow 103 5 2 Semi Micro Flow Cell 103 A 5 3 Semi Preparative Flow Cell 104 Doc 031898 03 3 06 iii PDA 100 USB Photodiode Array Detector A 6 104 B Installation B 1 B 2 B 3 Facilities Required cece ees 107 Unpacking the PDA 100 107 Installation A Age BE Ah Rod t AA Oa 108 B 3 1 Before You
49. ating absorbance 48 Calibration wavelength 24 85 Caution icon 6 Cells 13 14 41 Air bubble prevention 74 114 Air bubble removal 89 Doc 031898 03 3 06 Index 1 PDA 100 USB Photodiode Array Detector Backpressure line 74 Backpressure line installation 114 Chemical compatibility 41 Cleaning procedure 89 Contaminants 74 Heat exchangers 15 17 88 104 Illustration 15 17 113 Installing 112 Leaks 11 Path length 103 105 Specifications 103 Stains on cell interior 93 Chromeleon software 1 23 2D Control panel 30 33 3D Control panel 30 32 33 3D Data Acquisition license 1 3 30 33 Audit Trail 9 11 57 84 Automated control mode 23 Commands dialog box 23 Diagnostic procedures 85 Direct control mode 23 30 32 Installation instructions 108 PDA 100 commands 23 24 PDA 100 Wellness panel 85 86 Peak purity analysis 1 PGM files 23 PGM Wizard 23 33 USB driver information 108 Commands dialog box 23 Components elute slowly 74 D Danger icon 6 Dark signal 13 Data collection rate 23 41 Correlation with rise time 43 Definition 43 Guidelines for selecting 43 Relationship to step 49 Data files occupy too much disk space 43 Data points 24 43 49 Minimum number per peak 43 Data Processing board 19 115 Analog output connectors 19 Lithium battery disposal 87 Deuterium lamp 12 13 Age command 24 Calibration
50. avelength 24 86 Visible focus lens 13 Visible wavelengths 13 Vorsicht icon 7 W Warning icon 6 Warnung icon 7 Warranty voiding 87 Waste line 22 Installation 114 Wavelength calibration 1 24 80 85 Causes of failure 80 91 Result 24 Wavelength verification 13 24 80 86 Result 24 Wavelengths single 1 44 Reference modes 45 Windows cell 13 Contamination 80 91 Cracked 93 Etching with strong bases 14 25 41 Replacement kit 91 Replacement procedure 91 92 Doc 031898 03 3 06 Index 7 PDA 100 USB Photodiode Array Detector Index 8 Doc 031898 03 3 06
51. bs 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 4 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 e 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 031898 03 3 06 83 PDA 100 USB Photodiode Array Detector 4 14 Faulty USB Communication PDA 100 not recognized by Windows operating system Dionex strongly recommends installing Chromeleon before connecting the PDA 100 to the computer When the software is installed first USB driver information is loaded automatically If you connect the PDA 100 to the computer before installing Chromeleon a Windows message box requesting a USB configuration file cmwdmusb inf will appear when you turn on the computer Follow these steps to resolve the problem 1 Click Cancel in the Windows message box 2 Turn offthe power to the PDA 100 and unplug the USB cable from the computer 3 Install Chromeleon 4 Reconnect the USB cable to the computer and turn on the power to the PDA 100 Windows will now automatically recognize the detector 4 15 Diagnostics 4 15 1 Moduleware Run Time Diagnostics The PDA 100 Moduleware periodically checks the
52. c NOTE When the reference wavelength is off the reference bandwidth is not used The reference value is the first data point of the sample wavelength and bandwidth after autozero 10 To program 3DFIELD the 3D channel a Check or clear the check box to determine whether 3D data will be collected b Ifthe channel is selected enter the starting and ending data acquisition times as well as the reference wavelength and reference bandwidth NOTE 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 11 Enter the 3D Min Wavelength and 3D Max Wavelength NOTE If the data collection rate is 20 Hz the 3D sample wavelength range must be lt 310 nm 12 Enter the 3D Bunchwidth the distance between wavelengths 13 Click Next to continue Doc 031898 03 3 06 37 PDA 100 USB Photodiode Array Detector The following screen is displayed The tree control lists states for all devices in the selected timebase Click the plus sign to the left of a device name to expand or collapse the structure and view the device states Program Wizard Relay and State Devices Options x E Pump_ColumnValve Retention Time min Add H Pump InjectValve E Pump Relay 1 State Open Delete Pump Relay 2 Pune TT
53. can change the severity level assigned to a problem whenever appropriate Icon Severity Level Description Warning A message is displayed in the Audit Trail 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 031898 03 3 06 57 PDA 100 USB Photodiode Array Detector The table below lists the PDA 100 error messages and their default severity levels For troubleshooting assistance refer to the page indicated in the table 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
54. d 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 PDA 100 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 the analog recorder outputs Doc 031898 03 3 06 19 PDA 100 USB Photodiode Array Detector 2 5 Rear Panel Figure 2 7 illustrates the rear panel of the PDA 100 eee Fuse Holder Main Power Receptacle USB Analog Outputs Relay TTL dens Connectors Connector Figure 2 7 PDA 100 Rear Panel Power Entry The PDA 100 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 SHOCK HAZARD To avoid electrical shock use a grounded receptacle Do not operate the PDA 100 or connect it to AC power mains without an earthed ground connection
55. 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 Valid steps are 0 05 0 1 0 2 0 4 0 5 1 2 and 4 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 60 page 62 page 62 page 62 page 62 page 63 page 63 page 63 page 63 page 63 page 64 page 64 page 64 page 65 page 65 page 65 page 66 page 66 page 66 page 67 page 67 58 Doc 031898 03 3 06 4 Troubleshooting Alarms and Error Conditions Default Severity See Level The minimum wavelength must be less than the Error page 67 maximum wavelength Min wavelength X max wavelength X The range of wavelength bunching is 1 to 25 nm Error page 67 The range of wavelengths is outside the 190 to 800 nm Error page 68 limit Wavelength X Bandwidth X UV lamp control circuitry error while lamp is off Abort page 70 UV lamp error or control circuitry error while lamp is on Abort page 68 UV lamp error Abort page 68 UV lamp error while attempting to turn off Abort page 68 UV lamp error while attempting to turn on Abort page 68 UV lamp fa
56. e 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 5 Flush the cell with deionized water for 20 to 30 minutes at 1 0 mL min 5 3 Removing Trapped Air from the Flow Cell Trapped air bubbles in the flow cell may cause pulsations of the baseline or random noise 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 Usinga 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 031898 03 3 06 89 PDA 100 USB Photodiode Array Detector 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 PDA 100 front panel by the sides and pull straight off to remove 2 Disconnect the tubing connected to the flow cell inlet and outlet see Figure 5 1 3 Remove the flow cell cover from the inside front panel see Figure 2 2 4 Standard or semi micro cell Remove the tubing bracket from the lamp cover see Figure 5 1 5 Remove the flow cell inlet tubing from
57. e on the lamp cover and reinstall the tubing bracket see Figure 5 1 4 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 5 Push the detector front panel into place Doc 031898 03 3 06 93 PDA 100 USB Photodiode Array Detector 5 7 Replacing the Deuterium Lamp 1 Stop the Chromeleon server 2 Turn off the PDA 100 power switch 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 gt gt 2 2 AVERTISSEMENT 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 gt WARNUNG 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 gt CAUTION 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 gt MISE EN GARDE Das Lampengehause und die Lampenbefestigung k nnen sehr hei werden bes
58. e replaced see Section 5 5 Do not use a PEEK flow cell with normal phase or chlorinated IMPORTANT solvents these solvents will damage the cell Doc 031898 03 3 06 41 PDA 100 USB Photodiode Array Detector Do not use a stainless steel flow cell with low pH solutions these IMPORTANT or solutions may cause corrosion contamination and metal leaching Rise Time Rise time is a measure of how quickly the PDA 100 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 PDA 100 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 longer rise time allows more averaging of the signal and results in less short term noise see Figure 3 3 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 Rise Time 0 5 sec Baseline Noise 22 AU Tv WVL 254 nm MW I iy M JM y N M m 0 01004 0 00 Rise Time 2 0 sec Baseline Noise 10 AU om SAT WVL 254 nm 1 d il A Al h I d Sr ON dir NM d Ji W l A hy AM ah Nay Wl TIT 0 0100 NK 4 i m i T T 0 00 1 00 2 00 3 00 4 00 5 00
59. ead connector on the side wall see Figure 5 3 9 Usea 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 10 Inspect the new tungsten lamp P N 0561237 for fingerprints and dust If necessary clean the lamp with IPA isopropyl alcohol Doc 031898 03 3 06 97 PDA 100 USB Photodiode Array Detector 11 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 12 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 13 Replace the lamp cover IMPORTANT Do not pinch the Vis lamp connector wires under the lamp cover 14 Thread the cell inlet tubing through the tubing guide on the lamp cover and reinstall the tubing bracket 15 Replace the flow cell cover and reconnect the inlet and outlet tubing IMPORTANT Do not pinch the tubing under the flow cell cover 16 Replace the detector front panel 17 Turn on the detector power 18 Start the Chromeleon server 19 Resetthe lamp lifetime a Press F8 to display the Commands dialog box b Select UV and select VisLampA
60. ection provides a brief overview of detector control For complete operating instructions refer to the Chromeleon online Help or user s guide 1 Start the Chromeleon Server by double clicking the Server Monitor icon on the taskbar 2 Start Chromeleon by selecting Start gt Programs gt Chromeleon gt Chromeleon The main window and the Browser will appear 3 In the Browser expand the Dionex Templates Panels Dionex_IC PDA 100 USB folder The folder contains two default Control panels e DIONEX PUMP PDA AUTOSAMPLER PAN the 2D panel monitors chromatograms of up to five signals see Figure 3 1 e DIONEX PUMP PDA3D AUTOSAMPLER PAN the 3D panel monitors chromatograms contour plots and spectra online see Figure 3 2 NOTE The 3D Control panel is not available unless Chromeleon includes the 3D Data Acquisition license Doc 031898 03 3 06 33 PDA 100 USB Photodiode Array Detector Creating a New PGM File Careful selection of the data collection rate rise time and other operating parameters will optimize the performance of the PDA 100 Before creating a PGM file you may want to review Section 3 3 for a description of these parameters how they interact with each other and some guidelines for their selection 1 Select File gt New A dialog box appears 2 Select Program File and click OK The initial Program Wizard screen is displayed Program Wizard Select Timebase Options x The Program Wizard
61. ed 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 Doc 031898 03 3 06 21 PDA 100 USB Photodiode Array Detector 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 2 2 The analog outputs continue to output data even after the computer running Chromeleon is turned off or is disconnected from the PDA 100 When the detector power is turned on again the analog output settings will be either the factory defaults see Section 3 4 or the settings selected the last time the detector was controlled by the computer 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 PGM file see Section 3 2 2 in Chromeleon or controlled manually through a Control panel in the software The Relay out
62. ee 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 112 Doc 031898 03 3 06 B Installation 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 4 d Cell Outlet Tubing Reducing Union Fitting IB PEEK cell P N 055903 Cell Inlet Tubing Stainless steel cell P N 055902 Reducing Union Fitting VD PEEK cell P N 055903 Stainless steel cell P N 055902 Heat Exchangers Spring Clip Figure B 4 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 5 Cell Outlet Tubing Union Fitting 0 51 mm 0 020 in ID PIN 042627 P N 042855 Handle S Union Fitting f Spring Clip PIN 042627 Cell Inlet Tubing ff 0 51 mm 0 020 in ID P N 042855 Flow Cell Figure B 5 Semi Preparative Flow Cell Connections Doc 031898 03 3 06 113 PDA 100 USB Photodiode Array Detector IMPORTANT 9 10 Connect a length of 0 51 mm 0 020 in ID tubing P N 052309 to the cell outlet connection see Figure B 4 or Figure B 5 This is a waste line Connect a backpressure
63. efer 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 51 Drifting Baseline Fluctuations in ambient temperature Make sure the PDA 100 installation site temperature remains consistent Allow at least 6 cm 2 4 in of clearance behind the PDA 100 for ventilation Check that the flow cell inlet tubing is routed through the heat exchanger see Figure 2 4 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 45 Front panel lamp cover or flow cell cover is missing Optical components are sensitive to temperature and light Do not operate the PDA 100 unless the front panel lamp cover and flow cell cover are in place Flow cell 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 76 Doc 031898 03 3 06 4 Troubleshooting 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 install
64. elength 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 min Reference Wavelength Mode Active Baseline Drift 40 AU hour EE Pred 4ONoise0 48e0 m i WSS Figure 3 5 Effect of Reference Wavelength on Baseline Drift Doc 031898 03 3 06 47 PDA 100 USB Photodiode Array Detector Reference 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 a range surrounding the reference wavelength It is not necessary to select a reference bandwidth unless you enter a reference wavelength 1 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 e Select a reference bandwidth in an area of the spectrum where the sample does not absorb e 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 Example Chromatogram Selecting
65. ersonnel To contact Dionex in the U S call 1 800 346 6390 and select the Technical Support option Outside the U S call the nearest Dionex office NOTE The PDA 100 electronics are not user serviceable All repairs of the detector electronics must be performed by Dionex personnel Ze The Data Processing board contains a lithium battery If the board is F gt 4 di replaced dispose of the used battery according to local regulations or n Peng Before replacing any parts review the troubleshooting information in Chapter 4 to isolate the cause of the problem IMPORTANT Substituting non Dionex parts may impair the performance of the PDA 100 thereby voiding the product warranty Refer to the warranty statement in the Dionex Terms and Conditions for more information Doc 031898 03 3 06 87 PDA 100 USB Photodiode Array Detector 5 1 Liquid Leaks The PDA 100 is plumbed with the components listed in the tables below For tightening requirements refer to Installation of Dionex Ferrule Fittings The tubing connected to the heat exchangers standard and semi micro cells only as well as the inlet and outlet tubing on the semi preparative cell cannot be replaced If a leak at the cell inlet for example cannot be eliminated by tightening the fitting the entire cell must be replaced see Section 5 6 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 m
66. ervice and parts replacement procedures that users may perform Lists the PDA 100 specifications and installation site requirements Describes how to install the PDA 100 Lists spare parts for the PDA 100 Doc 031898 03 3 06 PDA 100 USB Photodiode Array Detector 1 4 Safety and Regulatory Information 1 4 1 gt DANGER gt WARNING gt CAUTION IMPORTANT d DANGER gt AVERTISSEMENT gt MISE EN GARDE Safety Messages This manual contains warnings and precautionary statements that can prevent personal injury and or damage to the PDA 100 when properly followed Safety messages appear in bold type and are accompanied by icons as shown below Indicates an imminently hazardous situation which if not avoided will result in death or serious injury Indicates a potentially hazardous situation which if not avoided may result in death or serious injury Indicates a potentially hazardous situation which if not avoided may result in minor or moderate injury Indicates that the function or process of the instrument may be impaired Operation does not constitute a 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 mortelles Signale une situation de danger potentiel qui si elle n est pas vit e pourrait entrainer des blessures graves mortelles Signale une situatio
67. f pyrene and the impurity see Figure 1 2 clearly indicate that the two peaks are different components Doc 031898 03 3 06 PDA 100 USB Photodiode Array Detector 1 Calibration 5 Solvent Injection 2 Calibration 4 modified by bclemons UV VIS 1 15 0 10 0 5 0 3 231 3 375 3 500 3 625 3 750 3 957 Figure 1 1 Overlay of Pyrene and an Impurity Calibration 4 Compound Mix 20 0 pl Pyren 3 51 60 0 Pyren 3 52 Impurity Pyrene 4 20 0 10 0 200 250 300 350 400 450 500 595 Figure 1 2 Spectra of Pyrene and an Impurity 4 Doc 031898 03 3 06 1 Introduction 1 3 Overview of This Manual Chapter 1 Introduction Chapter 2 Description Chapter 3 Operation and Maintenance Chapter 4 Troubleshooting Chapter 5 Service Appendix A Specifications Appendix B Installation Appendix C Reordering Information Introduces the PDA 100 and the theory of photodiode array detection explains the conventions used in this manual including safety related information Provides an overview of PDA 100 operating features and system components Provides an overview of PDA 100 operation including guidelines for optimizing detector performance describes routine preventive maintenance procedures Lists problems and presents step by step procedures for how to isolate and eliminate the cause of each problem Provides step by step instructions for routine s
68. fter a new deuterium lamp is installed Run the wavelength calibration and wavelength verification test for the new lamp see Section 4 15 2 96 Doc 031898 03 3 06 5 Service 5 8 Replacing the Tungsten Lamp 1 Stop the Chromeleon server 2 Turn off the PDA 100 power switch 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 apr s 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 3 Grasp the detector front panel by the sides and pull straight off to remove 4 Standard or semi micro cell Remove the tubing bracket from the lamp cover see Figure 5 1 5 Remove the flow cell inlet tubing from the tubing guide in the lamp cover see Figure 5 1 6 Remove the flow cell cover from the inside front panel see Figure 5 1 7 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 8 Squeeze the clip on the visible lamp connector and disconnect it from the 4 pin bulkh
69. ge c Resetthe lamp age to zero d Click Execute NOTE Before resuming routine operation allow 20 to 30 minutes for the lamp to stabilize 98 Doc 031898 03 3 06 5 Service 5 9 Replacing the Main Power Fuses DANGER DANGER ACHTUNG HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the PDA 100 HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du PDA 100 HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite des PDA 100 Turn off the PDA 100 power switch Disconnect the power cord from the PDA 100 rear panel The fuse holder 15 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 screwdriver and twist to release each side compartment Fuse Holder Fuses 2 ocking Spring Locking d P Serna P Insert Fuse Holder Side View Main Power Receptacle Figure 5 4 Main Power Fuse Holder Doc 031898 03 3 06 99 PDA 100 USB Photodiode Array Detector 4 Replace the two fuses in the holder with new 4 0 amp fast blow IEC 12
70. guides you through the creation of program files To start select the timebase where the program will run Timebase s ystem 1 Computer _1 Protocol My Computer 2 Enter connection information manually or pick a timebase from the list at right My Computer System_1 Favorites Network Neighborhood ERC 3 Select the Timebase where the program will run 4 Click Next to continue 34 Doc 031898 03 3 06 3 Operation and Maintenance If the selected timebase includes other devices pump autosampler etc Program Wizard screens for these devices precede the PDA 100 screens Click the Next button on each screen until the Acquisition Options screen appears Program Wizard Acquisition Options Acquisition Time From 0 000 min To 30 000 min Select data acquisition channels devices vuv Select All Deselect All te ee 5 To determine for how long data will be collected specify when the Acquisition Time starts and ends 6 Select the channels and or devices for which data will be collected To enable or disable all entries listed here click Select All or Deselect All respectively 7 Click Next to continue Doc 031898 03 3 06 35 PDA 100 USB Photodiode Array Detector The following screen is displayed Program Wizard UY Options x Data Collection Rate 2 00 D 0 25 20 00 Hz Rise Time 2 00 0 05
71. he baseline may shift This mode also helps compensate for fluctuations in ambient temperature caused by air conditioning NOTE Ifthe active reference mode is selected 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 see page 37 If the data collection rate is 20 Hz the 3D sample wavelength range must be lt 310 nm see page 43 To cancel the active reference mode enter Off as the reference wavelength The intensity reading at the time of autozero will be used as 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 46 Doc 031898 03 3 06 3 Operation and Maintenance Example Chromatogram Selecting the Reference Wavelength Figure 3 5 shows the results obtained from two different channels within the same run When the reference wavelength mode is Off Ge the active reference mode is cancelled the baseline drift is 120 AU hour When the active reference mode is selected the baseline drift is reduced to 40 pAU hour The operating conditions are Sample wav
72. hoot This message appears if the PDA 100 fails to respond when the computer attempts to communicate with the detector Shut down the Chromeleon server and turn off the PDA 100 power wait 30 seconds and then power up both the server and the detector If the error message appears again contact Dionex for assistance 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 PDA 100 power for 30 seconds and then turn it on again If the error message appears again contact Dionex for assistance 64 Doc 031898 03 3 06 4 Troubleshooting Filter wheel sensor could not detect blocked position Filter wheel sensor could not detect open position A backup paddle alignment routine ensures that the PDA 100 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 if desired To troubleshoot 1 Turn off the PDA 100 power for 30 seconds and then turn it on again 2 Ifthe error message appears again check the deuterium lamp intensity a In Chromeleon press
73. hub to the PC Contact Dionex to order the external hub P N 060392 and USB cable P N 960779 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 Doc 031898 03 3 06 109 PDA 100 USB Photodiode Array Detector 1 Plug the A connector of a USB cable P N 960779 into a port on the external USB hub P N 060392 You may use either the cable provided in the PDA 100 Ship Kit or the extra cable ordered for this configuration Plug the B connector of the cable into the USB receptacle on the PDA 100 rear panel see Figure B 2 Plug the A connector of a USB cable P N 960779 into a USB port on the computer on which Chromeleon is installed Plug the B connector of the cable into a port on the USB hub see Figure B 2 Plug the USB cable s B connector into the USB receptacle on the PDA 100 Plug the USB cable s A connector into the A port on the USB hub PDA 100 Chromeleon Computer Plug the USB cable s A connector into the USB port on the PC Plug the USB cable s B connector into the B port on the USB hub B 3
74. iled to turn on for the required operation Abort page 68 Visible lamp control circuitry error while lamp is off Abort page 70 Visible lamp error or control circuitry error while lamp is Abort page 68 on Visible lamp error Abort page 68 Visible lamp error while attempting to turn off Abort page 70 Visible lamp error while attempting to turn on Abort page 68 When collecting at 20Hz the spectrum range cannot be Abort page 70 more than 310 nm Please lower the data rate or narrow the spectrum range Doc 031898 03 3 06 59 PDA 100 USB Photodiode Array Detector 3DFIELD RefWavelength and or RefBandwidth is out of range To troubleshoot For all data collection rates other than 20 Hz select parameters that meet the following criteria 190 lt A 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 60 Doc 031898 03 3 06 4 Troubleshooting When the data collection rate is 20 Hz select parameters that meet the following cr
75. inched under the lamp cover 3 Check the number of hours the lamp has been in service In Chromeleon press F8 to display the Commands dialog box and select UV If the error message relates to the deuterium lamp select the UVLampAge command 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 Dionex for assistance If the deuterium lamp has been in operation for less 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 select 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 Dionex for assistance If the tungsten lamp has been in operation for ess than 2000 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 031898 03 3 06 69
76. 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 front panel LED Deuterium or Tungsten is lighted 74 Doc 031898 03 3 06 4 Troubleshooting 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 e Inappropriate reference wavelength Select a reference wavelength in a quiet area of the spectrum where little absorption occurs Dionex recommends selecting a reference wavelength below 380 nm for UV applications and above 600 nm for visible applications For more information see page 45 e Bandwidth is too narrow Select a wider bandwidth and reference bandwidth if appropriate for
77. ing 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 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 page 48 Dionex recommends selecting a reference wavelength 1 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 page 45 4 7 Deuterium Lamp Intensity Reading Too Low Light signal is not reaching the data processor Check that at least one lamp is turned on When a lamp is on the corresponding front panel LED Deuterium or Tungsten is lighted If necessary turn on one of the lamps from either 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 In Chromeleon press F8 to display the Commands dialog box b Select UV and then select LampIntensity Doc 031898 03 3 06 77 PDA 100 USB Photodiode Array Detector
78. ing is acceptable and the Power LED is no longer flashing resume normal operation If the reading is acceptable but the Power LED is still flashing contact Dionex for assistance If the reading is too low follow the troubleshooting steps in Section 4 7 4 3 Lamp Does Not Light or Lamp LED Is Flashing 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 from the TTL input To restore the default setting for a lamp 1 Press F8 in Chromeleon to display the Commands dialog box and select UV 2 Select UVLampPowerOnSetting for the deuterium lamp and click Execute 3 Select VisLampPowerOnSetting for the tungsten lamp and click Execute 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 4 4 No Detector Response Detector power not on Check that the power cord is connected from the PDA 100 rear panel to a power source Check that the main Power switch is turned on Check the fuses and replace them if necessary see Section 5 9 72 Doc 031898 03 3 06 4 Troubleshooting 4 5 Lamp not turned on Turn on the lamp from either Chromeleon or the TTL input When a lamp is on the
79. installed 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 114 Doc 031898 03 3 06 B Installation B 3 7 B 3 8 gt CAUTION gt WARNING gt AVERTISSEMENT gt WARNUNG Making the Analog Output Connections Connect a recorder an integrator or an A D data acquisition device to the ANALOG OUT connector on the PDA 100 rear panel see Figure B 3 The four PDA 100 analog outputs provide a 1 volt output maximum The outputs are controlled by absorbance wavelengths 1 through 4 in Chromeleon The software controls the wavelength sample bandwidth reference wavelength full scale absorbance output and offset within the 0 to 1 volt range Making the Relay TTL Connections 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 LECTROCUTION ET 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 wi
80. ion of the PDA 100 follow these steps Press the Power switch on the front panel to turn on the detector see Figure 2 1 e Verify that the Power LED is lighted e Verify that the Deuterium and or Tungsten LEDs are lighted e 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 031898 03 3 06 29 PDA 100 USB Photodiode Array Detector 3 2 Routine Operation 3 2 1 Direct Control In the direct control mode PDA 100 commands and operating parameters are selected from the Chromeleon menu bar toolbars and Control panels Direct control commands are executed as soon as they are entered Parameters can be modified at any time during manual data acquisition NOTE This section provides a brief overview of detector control For complete operating instructions refer to the Chromeleon online Help or user s guide Start the Chromeleon Server by double clicking the Server Monitor icon on the taskbar Start Chromeleon by selecting Start gt Programs gt Chromeleon gt Chromeleon The main window and the Browser will appear In the Browser expand the Dionex Templates Panels Dionex_IC PDA 100 USB folder The folder contains two default Control panels e DIONEX PUMP PDA AUTOSAMPLER PAN the 2D panel monitors chromatograms of up to five signals see Figure 3 1 e DIONEX PUMP PDA3D
81. ions 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 pistons remove the pistons and IMPORTANT SENE 3 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 IMPORTANT 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 Doc 031898 03 3 06 27 PDA 100 USB Photodiode Array Detector 28 Doc 031898 03 3 06 3 Operation and Maintenance The PDA 100 Photodiode Array Detector is designed for use with IC 1on chromatography BioLC biocompatible liquid chromatography and HPLC high performance liquid chromatography systems and should not be used for any other purpose Operation of the PDA 100 in a manner not specified by Dionex may result in personal injury If you have a question regarding appropriate usage contact Dionex before proceeding In the U S call 1 800 346 6390 and select the Technical Support option Outside the U S call the nearest Dionex office 3 1 Getting Started Before beginning operat
82. is off Tungsten Lighted The tungsten lamp is on Flashing A command was issued to turn on the tungsten 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 detector power is on Press the Power switch for on off control of the detector Flashing The detector failed the start up routine see Section 4 2 Off The detector power is off Press the Power switch for on off control of the detector Table 2 1 PDA 100 Front Panel LEDs 10 Doc 031898 03 3 06 2 Description 2 2 Inside Front Panel Grasp the PDA 100 front panel by the sides and pull it straight off to access the inside front panel see Figure 2 2 Flow Cell Cover Figure 2 2 PDA 100 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 are not immediately apparent 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 whe
83. iteria Minimum lt A lt Maximum A Maximum Minimum A lt 310 nm Where Reference wavelength 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 Doc 031898 03 3 06 61 PDA 100 USB Photodiode Array Detector 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 Dionex if you want to order this option Autozero is already in progress To troubleshoot This message appears if you select Autozero in the 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 calibra
84. l 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 O ring from sealing IMPORTANT z 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 031898 03 3 06 91 PDA 100 USB Photodiode Array Detector IF Cell Outlet Tubing 4 Cell Inlet Tubing O Ring Groove 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
85. lems Leak sensor error To troubleshoot Locate the source of the leak First tighten or replace all liquid line connections If the connections are made with Dionex ferrule fittings refer to Installation of Dionex Ferrule Fittings for tightening requirements 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 66 Doc 031898 03 3 06 4 Troubleshooting Over temperature 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 PDA 100 power and contact Dionex for assistance NOTE Do not attempt to service the PDA 100 electronics components All repairs of the electronics components must be performed by Dionex personnel PDA is running a calibration or diagnostic function Not ready to accept this command To troubleshoot Wait until the calibration 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 minimu
86. 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 PDA 100 Ship Kit 0 25 mm 0 010 in ID tubing P N 052306 two ferrule fittings P N 043276 and two 10 32 bolts P N 043275 b 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 c Install a ferrule fitting and 10 32 bolt on each end of the tubing d Connect the backpressure line to the waste line installed in Step 9 Use a union P N 042627 to connect the backpressure line to the waste line 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 12 13 Thread the cell outlet tubing through the slot near the bottom of the front panel Thread the cell inlet tubing through the slot on the right side Push the detector front panel into place Connect the cell inlet tubing to the separator column outlet B 3 6 Connecting the Waste Line Connect the waste line P N 054779 to the PDA 100 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 PDA 100 is
87. ls Av Alternating current D Protective conductor terminal Power supply is on Doc 031898 03 3 06 PDA 100 USB Photodiode Array Detector Power supply is off Indicates a potential hazard Refer to the operator s manual for an explanation of the hazard how to proceed 8 Doc 031898 03 3 06 2 Description 2 1 Front Panel Figure 2 1 illustrates the PDA 100 Photodiode Array Detector front panel e Press the Power switch in the lower left corner for on off control of the detector power e The four LED indicators identify the status of the detector power the deuterium and tungsten lamps and the analysis see Table 2 1 When the corresponding function is in progress the LED is lighted If an error occurs the LED flashes and an error message 1s logged in the Chromeleon Audit Trail Figure 2 1 PDA 100 Photodiode Array Detector Doc 031898 03 3 06 9 PDA 100 USB Photodiode Array Detector LED LED Status Function Run Lighted Data is being acquired by Chromeleon Flashing The leak sensor in the drip tray was triggered Off Data is not being acquired by Chromeleon Deuterium Lighted The deuterium lamp is on Flashing A command was issued to turn on the deuterium 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 deuterium lamp
88. m 0 015 in ID P N 057304 N A 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 1 PDA 100 with Standard Cell Component PEEK Cell SST Cell 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 2 PDA 100 with Semi Micro 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 Table 5 3 PDA 100 with Semi Preparative Cell 88 Doc 031898 03 3 06 5 Service 5 2 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 syring
89. m 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 to 25 nm Doc 031898 03 3 06 67 PDA 100 USB Photodiode Array Detector The range of wavelengths is outside the 190 to 800 nm limit To troubleshoot The PDA 100 can measure the absorbance spectrum from 190 to 800 nm Make sure both the minimum and maximum wavelengths are within this range 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 front panel LED Deuterium or Tungsten is lighted If necessary turn on the lamp from either Chromeleon or the TTL input 68 Doc 031898 03 3 06 4 Troubleshooting 2 Ifyou 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 p
90. mbly 042627 Union fitting 043276 Ferrule 043275 Nut 118 Doc 031898 03 3 06 Numerics 2D data acquisition 2D Control panel 33 2D data collection 1 36 2D Control panel 30 3D Data Acquisition license 1 3 30 33 Error message 58 62 3D data collection 23 37 3D Control panel 30 32 3D Data Acquisition license 1 3 30 33 Bunch width selection 49 Reducing data file size 50 Step time selection 50 A Absorbance calculation 48 Absorbance range 22 Achtung icon 7 Active reference mode 45 46 See also Reference wavelength Selecting 76 Turning off 46 Turning on 45 Air bubbles in cell Preventing 74 114 Removing 89 Air conditioning 46 Ambient temperature fluctuations 46 Analog output connectors 1 19 22 115 Default settings 53 Output 115 Analog output range 22 Analytes unknown 44 Audit Trail 9 11 57 Average 41 Definition 51 Index Guidelines for selecting 51 Avertissement icon 6 B Backpressure 54 Increase 54 Backpressure line 74 Installation 114 Bandwidth 23 41 Definition 44 Guidelines for selecting 44 Setting is too narrow 75 Baseline drift 41 47 Causes 91 Reducing 46 Troubleshooting 76 77 Baseline noise 41 Causes 80 89 91 Reducing 42 44 46 48 83 Relationship to rise time 42 Bolts 10 32 114 Bunch width 23 41 Definition 49 Guidelines for selecting 49 C Cable USB 110 Installation 109 110 Part number 117 Calcul
91. n de danger potentiel qui si elle n est pas vit e pourrait entrainer des blessures mineures mod r es galement utilis pour signaler une situation ou une pratique qui pourrait gravement endommager l instrument mais qui n entrainera pas de blessures Doc 031898 03 3 06 1 Introduction ACHTUNG WARNUNG VORSICHT 1 4 2 Warnhinweise in Deutsch Bedeutet unmittelbare Gefahr Mi amp achtung kann zum Tod oder schwerwiegenden Verletzungen f hren Bedeutet eine m gliche Gef hrdung MiRachtung kann zum Tod oder schwerwiegenden Verletzungen f hren Bedeutet eine m gliche Gefahrdung MiRachtung kann zu kleineren oder mittelschweren Verletzungen f hren Wird auch verwendet wenn eine Situation zu schweren Schaden am Gerat f hren kann jedoch keine Verletzungsgefahr besteht 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 Product Labels The TUV GS C US Mark safety label and the CE Mark label on the PDA 100 indicate that the PDA 100 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 These symbols appear on the PDA 100 or on PDA 100 labe
92. n test for both the deuterium and tungsten lamps approximately every 6 months see Section 4 15 2 If a lamp fails the test calibrate the wavelength see Section 4 15 2 and then run the wavelength verification test again If a lamp fails the test again replace it For lamp replacement instructions see Section 5 7 or Section 5 8 for the deuterium lamp or tungsten lamp respectively Doc 031898 03 3 06 55 PDA 100 USB Photodiode Array Detector 56 Doc 031898 03 3 06 4 1 4 Troubleshooting This chapter is a guide to troubleshooting problems that may occur while operating the PDA 100 Photodiode Array Detector 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 15 describes some of the diagnostic features available in the PDA 100 Moduleware and Chromeleon software If you are unable to eliminate a problem contact Dionex In the U S call 1 800 346 6390 and select the Technical Support option Outside the U S call the nearest Dionex office Alarms and Error Conditions The PDA 100 Moduleware periodically checks the status of certain system parameters If a problem is detected it is reported to the Chromeleon PC and displayed in the Chromeleon Audit Trail Each error message is preceded by an icon that identifies the seriousness of the underlying problem see the table below You
93. n wet When the leak sensor is activated it triggers an alarm in the detector and the front panel Run LED begins flashing see Figure 2 1 In addition the leak is reported to Chromeleon and an error message is logged in the Audit Trail Doc 031898 03 3 06 11 PDA 100 USB Photodiode Array Detector 2 3 Optical System Figure 2 3 is a schematic of the PDA 100 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 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 Di Lamp Deuterium Lamp Flow Cell Filter SSR A Photodiode gie SK At Lens 21 Spectrograph Lens Grating E i Figure 2 3 PDA 100 Optical System 12 Doc 031898 03 3 06 2 Description Optical System Component Tungsten Lamp Visible Focus Lens Deutertum Lamp Source Lens Flow Cell Spectrograph Lens Filter Paddle Slit Grating Photodiode Array Function The light source for visible and near infrared wavelengths 380
94. new deuterium lamp P N 939016T for fingerprints and dust If necessary clean the lamp with IPA isopropyl alcohol 11 Line up the 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 12 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 13 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 14 Replace the lamp cover IMPORTANT Do not pinch the UV lamp connector wires under the lamp cover Doc 031898 03 3 06 95 PDA 100 USB Photodiode Array Detector 15 16 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 17 18 19 20 2 Replace the detector front panel Turn on the detector power Start the Chromeleon server Reset the lamp lifetime a Press F8 to display the Commands dialog box b Select UV c Select UVLampAge d Reset the lamp age to zero e Click Execute NOTE It is normal for the baseline to drift for several hours a
95. ns are made with Dionex ferrule fittings refer to Installation of Dionex Ferrule Fittings for tightening requirements Doc 031898 03 3 06 73 PDA 100 USB Photodiode Array Detector 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 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 e Connect a backpressure line to the cell see Section B 3 5 This
96. nsity Select Autozero in the Commands dialog box and click Execute 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 Dionex for assistance Doc 031898 03 3 06 79 PDA 100 USB Photodiode Array Detector 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 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 b Ifthe error message appears again contact Dionex for assistance 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 PDA 100 Wellness panel and run the wa
97. 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 If tightening the retaining nut s stops the leakage dry the cell thoroughly with a lint free optical grade tissue and go on to Step 11 92 Doc 031898 03 3 06 5 Service 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 e If necessary 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 Dionex to order a new cell 11 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 Remove the flow cell from the optical bench see Section 5 4 2 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 3 Thread the flow cell inlet tubing through the tubing guid
98. odular power cord IEC 320 C13 from the PDA 100 main power receptacle see Figure B 3 to a grounded single phase power source Use the front panel Power switch to turn the detector on and off Fuse Holder Main Power Receptacle USB Analog Outputs Relay TTL de Connectors Connector Figure B 3 PDA 100 Rear Panel Doc 031898 03 3 06 111 PDA 100 USB Photodiode Array Detector B 3 5 IMPORTANT Installing the Flow Cell Do not touch the cell windows If you touch a window clean it with isopropyl alcohol IPA and a clean lens tissue 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 leaching Grasp the PDA 100 front panel by the sides and pull straight off to remove Remove the flow cell cover from the inside front panel see Figure 2 2 Standard or semi micro cell Remove the tubing bracket from the lamp cover see Figure 5 1 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 Thread the flow cell inlet tubing through the tubing guide on the lamp cover and reinstall the tubing bracket s
99. ol 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 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 the Data Collection Rate section on page 43 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 the Average section on page 51 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 50 Doc 031898 03 3 06 3 Operation and Maintenance Average The Average parameter operates in conjunction with the Step parameter see the Step section on page 49 When Average is On Chromeleon averages the data points between Step intervals reports that value and noise 1s reduced This setting is recommended for most applications When Average is Off Chromeleon 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 si
100. olutions will Compatibility etch the fused silica windows of the flow cell Do not use normal phase or chlorinated solvents with the flow cell these solutions will damage the cell A 6 Heat Exchangers Maximum PEEK cell 2 MPa 300 psi Operating Stainless steel cell 3 MPa 500 psi Pressure Volume of PEEK cell 45 uL Standard Cell Stainless steel cell 20 uL Heat Exchangers including cell inlet tubing 104 Doc 031898 03 3 06 A Specifications Volume of Semi PEEK cell 5 uL Micro Cell Heat Stainless steel cell 5 uL Exchangers including cell inlet tubing Doc 031898 03 3 06 105 PDA 100 USB Photodiode Array Detector 106 Doc 031898 03 3 06 B Installation B 1 Facilities Required e Make sure the PDA 100 installation site meets the power and environmental specifications listed in Appendix A Optical detectors are sensitive to vibrations Install the PDA 100 on a sturdy workbench in an environment that is vibration free e Allow at least 6 cm 2 4 in behind the PDA 100 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 Optical detectors are sensitive to changes in temperature and light Protect the PDA 100 the columns and all tubing connections from drafts Do not operate the PDA 100 unless the front panel lamp cover
101. onders wenn die Lampe l ngere Zeit in Betrieb war Warten Sie bis die Lampe abgek hlt ist bevor Sie diese ber hren gt VORSICHT 3 Grasp the detector front panel by the sides and pull straight off to remove 4 Standard or semi micro cell Remove the tubing bracket from the lamp cover see Figure 5 1 5 Remove the flow cell inlet tubing from the tubing guide in the lamp cover see Figure 5 1 6 Remove the flow cell cover from the inside front panel see Figure 5 1 7 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 8 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 94 Doc 031898 03 3 06 5 Service Flow Cell D Cover Deuterium Screw TT Lamp s Wire Guide UV Lamp Connector 6 pin Bulkhead Connector o 4 pin Bulkhead Connector Locating Tungsten Visible Lamp Connector Pin Red Power Lead Lamp N Leak Sensor Figure 5 3 Lamp Connections 9 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 10 Inspect the
102. psi Operating Stainless steel cell 3 MPa 500 psi Pressure Chemical e Do not use bases stronger than 0 1 M these solutions will Compatibility etch the fused silica windows of the flow cell 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 031898 03 3 06 103 PDA 100 USB Photodiode Array Detector Chemical e Do not use bases stronger than 0 1 M these solutions will Compatibility etch the fused silica windows of the flow cell 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 3 Semi Preparative Flow Cell Cell Body PEEK Volume and 0 7 uL volume 0 4 mm 0 02 in path length Optical Path Length Maximum 10 34 MPa 1500 psi Operating Pressure Chemical e Do not use bases stronger than 0 1 M these s
103. puts can be programmed to switch any low voltage control The switched current must be less than 200 mA and 42 V peak The PDA 100 Ship Kit P N 060977 includes a 12 pin connector P N 923686 for Relay and TTL connections For installation instructions see Section B 3 8 USB Connector The USB connector allows communication between the PDA 100 and the Chromeleon PC The PDA 100 is usually connected directly to the computer using a standard USB A to B cable P N 960779 For installation instructions see Section B 3 2 and Section B 3 3 Waste Line Waste exits the detector via a drain tube connected at the rear panel When correctly installed the drain tube is routed downward below the leak tray For installation instructions see Section B 3 6 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 detector 22 Doc 031898 03 3 06 2 Description 2 6 Chromeleon Software Chromeleon software is used to control PDA 100 operation Two modes of software control are available direct control and automated control e With direct control you select operating parameters and commands from the Chromeleon menu bar toolbars and Control panels see below Direct control commands are executed as soon as they are entered e With automated
104. r verifies wavelength calibration accuracy Five flow cells are available for standard semi micro and semi preparative applications The front panel LEDs indicate detector status at a glance e Four analog outputs support data collection on alternate data collection systems The PDA 100 is controlled remotely by a computer running the Chromeleon Chromatography Management System The detector communicates with the computer through USB Universal Serial Bus To take full advantage of the capabilities of the PDA 100 order Chromeleon with the 3D Data Acquisition license This license is required in order to perform e 3D data presentation and spectral analysis real time or post run Peak purity analysis with selectable criteria Doc 031898 03 3 06 1 PDA 100 USB Photodiode Array Detector 1 2 e Spectral library search for positive peak identification Each 3D Data Acquisition license applies to one chromatography server The total number of 3D data channels one server can acquire simultaneously depends on computer performance No special client license is required for reviewing and processing the 3D data acquired 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 PDA detectors scan a range of wavelengths every few milliseconds and continually genera
105. rd mit Netzspannung betrieben Der Service darf nur von qualifiziertem Personal durchgef hrt werden The PDA 100 Ship Kit includes a 12 pin connector P N 923686 for Relay and TTL connections see Figure B 6 To attach individual wires and twisted pairs to the connector strip the end of the wire s insert into the connector and tighten the locking screw s with a small screwdriver P N 046985 Doc 031898 03 3 06 115 PDA 100 USB Photodiode Array Detector RELAY OUT TTL TTLIN TTL OUT GND 1 2 1 121123 411 2 1234 5 6 7 8 9 10 1112 Figure B 6 Relay and TTL Connector The table below describes the pin assignments for the Relay and TTL connectors Relays 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 Pin Assignment Relay output Relay 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 TTL input or output O Ch tn BPW HA ra kon LA ra c Input Pin Function Active Ground Active Ground Active Active Active Autozero Active Reserved Active UV lamp on off Active Visible lamp on off Ground 1 Ground 2 116 Doc 031898 03 3 06 Part Number 939016T 056123T 954763 923686 043598 960779 056346 057304 055903 043276 043275 060498 056126 056124 055902 010262 0102
106. rformed by Dionex personnel e Tungsten LED is flashing The lamp did not power on properly Check the Chromeleon Audit Trail for a lamp related error message If necessary replace the lamp see Section 5 8 If the LED flashes again there may be a bad connection between the lamp power supply and the lamp Contact Dionex for assistance NOTE The PDA 100 electronics cannot be serviced by users All repairs of the electronics components must be performed by Dionex personnel Power LED is flashing If the Power LED starts flashing the first time the deuterium lamp is turned on the detector failed the start up routine Follow the steps below to resolve the problem 1 Remove the cell from the optical bench see Section 5 4 2 In Chromeleon press F8 to display the Commands dialog box and select UV 3 Select Autozero and click Execute to run the autozero routine If this corrects the problem the Power LED will stop flashing and you may replace the cell in the optical bench and resume normal operation If the Power LED continues flashing go on to Step 4 4 Checkthe deuterium lamp intensity a In Chromeleon press F8 to display the Commands dialog box b Select UV and then select LampIntensity The intensity reading should be above 10 million counts for a standard or semi Doc 031898 03 3 06 71 PDA 100 USB Photodiode Array Detector preparative cell or above 3 million counts for a semi micro cell If the read
107. s 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 031898 03 3 06 13 PDA 100 USB Photodiode Array Detector 2 3 4 Flow Cells Table 2 2 lists the flow cells available for use with the PDA 100 STANDARD FLOW CELLS Cell Material Cell CellPath 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 10mm 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 3 1 uL 9mm 5 ul Up to 1 0 mL min P N 064169 316 stainless steel 3 1 uL 9mm 5 ul Up to 1 0 mL min P N 064168 SEMI PREPARATIVE FLOW CELL Cell Material Cell CellPath Volume of Heat Intended Flow Volume Length Exchanger Rate Range Inlet Tubing PEEK 0 7uL 0 4mm N A 5 0 to P N 064167 100 0 mL min Table 2 2 PDA 100 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
108. s 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 PDA 100 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 031898 03 3 06 25 PDA 100 USB Photodiode Array Detector 2 8 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 baseline disruptions High sensitivity applications require a smooth low pulsation pump 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
109. t be changed Factory Default Settings The PDA 100 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 1s on A chart recorder or other voltage measuring device can be used to monitor the channels When the PDA 100 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 Wavelength 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 The following default settings are also in effect when the power is first turned on Rise time 2 0 seconds Lamp status The deuterium and tungsten lamps are on Stand Alone Operation The table below indicates which PDA 100 parameter each TTL input controls during stand alone operation TTL Input PDA 100 Parameter TTL 1 in Autozero TTL 2 in Reserved TTL 3 in Deuterium lamp on off TTL 4 in Tungsten lamp on off Doc 031898 03 3 06 53 PDA 100 USB Photodiode Array Detector 3 5 Routine Maintenance The following maintenance procedures may be performed by users All other maintenance procedures must be performed by Dionex personnel Before shutting down the detector for more than 24 hours flush the system with deionized water or methanol for at least 15 minutes at 1 0 mL min or maintain a
110. te spectral information Wavelength time and absorbance can all be plotted PDA detectors provide three dimensional information that allows an accurate assessment of peak identity purity and quantitation in a single analysis Software support for PDA detectors includes peak purity and spectral library search functions to help determine peak homogeneity and identity 1 2 1 Advantages of Photodiode Array Detection PDA detectors are useful in both research and quality assurance laboratories In the research laboratory the PDA provides the analyst with a variety of approaches to the analysis In the quality assurance laboratory the PDA provides several results from a single analysis thereby increasing the throughput of the HPLC PDA 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 PDA detector is used a wavelength range can be programmed and all compounds that absorb within this range can be detected in a single analysis Doc 031898 03 3 06 1 Introduction Determination of the correct wavelengths in one analysis After all peaks have been detected the maximum absorbance wavelength for each peak can be determined
111. tion procedure is in progress Wait until the procedure finishes 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 62 Doc 031898 03 3 06 4 Troubleshooting 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 PDA 100 power for 30 seconds and then turn it on again If the error message appears again contact Dionex for assistance 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 Doc 031898 03 3 06 63 PDA 100 USB Photodiode Array Detector is unavailable To troubles
112. uence OQ DAD WAVELENGTH Run Time 1 250 13 46 54 0 000 Sampler Got inject response i 48 54 0 000 UV VIS 1 AcqOn 13 46 54 0 000 3DFIELD AcgOn Uv2 1 7216 MAU any 2004 Sample Benzene hold benzene stop 1 250 3DFIELD AcqOrf System PDA 100 Signal 17 autosampler en EEN oero min 199 359 nm 1 nm Steps p Spectra 510 Autosampler Contour Plot rato Pump T 98 s08 mr 2 1612 mAU T 1 1 80 200 For Help press F1 start 4 EG server Coffiouration ch cnromeleon autosa Detector Signals for UV1 and UV2 Wavelengths SL m 10 Figure 3 2 PDA 100 3D Control Panel Example Click the Acquisition On Off toolbar button to stop manual data acquisition after the desired run time Data collected during the run may be saved to a sequence To retrieve the data select the assigned sample name within the sequence 32 Doc 031898 03 3 06 3 Operation and Maintenance 3 2 2 Automated Control A PGM file is a list of time precise control commands created by the user for automated operation of the PDA 100 PGM files can be created automatically with the help of the PGM Wizard or manually by editing an existing PGM file NOTE This s
113. velength calibration procedure see Section 4 15 2 No solvent flow through cell If the Power LED is flashing see Figure 2 1 flush the cell with deionized water or methanol and then turn off the detector power for 30 seconds Turn on the power again and verify that the Power LED is no longer flashing Check the 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 In Chromeleon press F8 to display the Commands dialog box and select UV 80 Doc 031898 03 3 06 4 Troubleshooting 2 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 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 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 65 for instructions 4 10 No Spectra Collected Spectral range was not programmed In Chromeleon select a spectral range in the PGM file or on
114. via the holmium oxide filter The result of the last wavelength verification test Doc 031898 03 3 06 2 Description 2 7 Mobile Phases Solvent quality significantly affects both detection limits and instrument performance To ensure optimal performance of the PDA 100 observe the following precautions Strong bases can etch the fused silica windows of the flow cell If the IMPORTANT i e 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 IMPORTANT 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 IMPORTANT e See a solutions may cause corrosion contamination and metal leaching Prepare all mobile phases with spectroscopy grade solvents reagent grade chemicals and ASTM Type I or better filtered deionized water 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 employ
115. wer 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 D INCENDIE Le module VAN 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 18 Doc 031898 03 3 06 2 Description 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 des potentiels DANGER D ELECTROCUTION Les composants utilis s pour allumer AN 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 adjuste
116. with a Dionex lon Chromatograph Document No 031883 The manual is available in two formats as a printed manual shipped with Chromeleon and as an Adobe PDF file on the Chromeleon CD ROM and the Dionex Reference Library CD ROM NOTE Dionex strongly recommends installing Chromeleon before connecting the PDA 100 to the computer on which Chromeleon is installed When Chromeleon is installed first USB driver information is loaded automatically 108 Doc 031898 03 3 06 B Installation B 3 2 Connecting the PDA 100 to the Chromeleon PC The PDA 100 is usually connected directly to a USB port on the computer on which Chromeleon is installed If a USB port is not available on the PC connect the PDA 100 to an external USB hub see Section B 3 3 1 Plug the A connector of a USB cable P N 960779 into the USB port on the computer see Figure B 1 2 Plugthe B connector ofthe USB cable into a USB receptacle on the PDA 100 rear panel USB Cable P N 960779 PDA 100 Plug the USB cable s Chromeleon connector into the USB Computer receptacle on the PDA 100 Plug the USB cable s A connector into the USB port on the PC Figure B 1 PDA 100 Connected Directly to the Chromeleon PC B 3 3 Connecting the PDA 100 to an External USB Hub If the PDA 100 cannot be connected directly to the Chromeleon PC see Section B 3 2 connect the detector to an external USB hub and then connect the
117. ws replacement procedure 91 92 Semi preparative flow cells 13 Chemical compatibility 104 Flow rate range 14 Doc 031898 03 3 06 Index 5 PDA 100 USB Photodiode Array Detector Heat exchanger volume 14 Operating pressure 104 Optical path length 14 104 Overview 14 Replacement procedure 93 See also Cells Volume 14 104 Windows replacement procedure 91 Sensitivity 41 Separator column 54 Service procedures Cell cleaning 89 Cell replacement 93 Cell window replacement 91 Deuterium lamp replacement 94 Electronics components 87 Eliminating liquid leaks 88 Fuse replacement 99 Removing air trapped in cell 89 Tungsten lamp replacement 97 Ship Kits PDA 100 107 Shutdown procedure 54 Signal intensity 46 Slit optical 12 13 Solvents Chlorinated 15 25 41 112 Normal phase 15 25 41 112 Source lens 12 13 Spare parts 117 Spectra not collected 81 Spectral library 2 3 Spectrograph lens 12 13 Spectrum 12 13 Improving resolution 81 Stainless steel flow cells 14 Cause of corrosion 15 25 42 103 104 112 Cause of metal leaching 15 25 42 104 112 Chemical compatibility 15 25 42 112 See also Cells Stainless steel systems Passivation 54 Standard flow cells 13 Chemical compatibility 103 Flow rate range 14 Heat exchanger volume 14 Operating pressure 103 Optical path length 14 103 Replacement procedure 93 See also Cells Volume 14 10
118. x select the entry and click Delete All entries in the list box will automatically be reorganized 18 Click Next to continue Doc 031898 03 3 06 39 PDA 100 USB Photodiode Array Detector The following screen is displayed Program Wizard Completion Completing the Program Wizard You now have entered all data required to create the program Please enter a title describing your program Now you can either save the program to disk immediately or review it and save it later C Save the program immediately Review the program in a new window Press Finish to open the program in a new window lt Back Finish Cancel f 19 Optional Type a descriptive Title for the program 20 Select one of the following options e To save the program without first reviewing it select Save the program immediately Clicking Finish opens a dialog box in which you can save the program e To review the program before saving it select Review the program in a new window Clicking Finish opens the program in the PGM Editor Use the PGM Editor to review the program and to manually edit it if necessary When you finish exit the PGM Editor This displays a prompt asking whether the program should be saved clicking Yes opens a dialog box in which you can save the program 40 Doc 031898 03 3 06 3 Operation and Maintenance 3 3 Optimizing Detector Performance The performance of the PDA 10
119. ze is more than double the rise time 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 PDA 100 becomes saturated when the light transmission is 20 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 Negative Absorbance Level 0 1 default 2 OQ HR Approximate Negative Absorbance at 210 nm 2200 mAU 2300 mAU 2600 mAU 2600 mAU 2700 mAU 2700 mAU 2700 mAU Approximate Negative Approximate Negative Absorbance at 240 nm Absorbance at 254 nm 50 mAU 100 mAU 200 mAU 300 mAU 400 mAU 500 mAU 600 mAU 300 mAU 350 mAU 450 mAU 550 mAU 630 mAU 660 mAU 760 mAU These signals are saturated and will not report a further negative value Doc

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