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PDA-100 Photodiode Array Detector Operator`s Manual

1. I CT D o 5 Q Flow Cell ei Cover Ri 6 5 U J O Leak Sensor A L Component Identification Label Figure 2 2 PDA 100 Inside Front Panel The flow cell cover protects the cell from dust ambient light fluctuations in ambient temperature and vibration The lamp cover enhances the thermal stabilization of the optical bench The optical bench is housed in a compartment behind the inside front panel 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 when wet If 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 the host computer and PeakNet 6 or Chromeleon displays an error message Doc 031644 02 9 03 2 3 PDA 100 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 tungste
2. 3 9 Optimizing Detector Performance 3 15 Stand Alone Analog Operation 3 28 Routine Maintenance 3 29 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 4 15 Flashing GED 2 Secs doe sat cites EE EEN EEN 4 1 No Detector Response 4 2 Noisy Baseline gt darane hoe te nad ered 4 3 Drifting 4 6 Lamp Does Not Light or Lamp LED Is Flashing 4 7 Deuterium Lamp Intensity Count Too 4 7 Wavelength Calibration Fals 4 8 Wavelength Verification Fails 4 9 Faulty DX LAN Communication 4 10 No Spectra Collected 4 10 Low Spectral Resolution 4 10 Peaks Too Large Small 4 11 Poor Peak Shape eene E De ep AN 4 12 Error Message Not Enough Light to Perform Operation 4 13 RIESEN 4 14 4 15 1 Moduleware Run Time Diagnostics 4 14 Doc 031644 02 9 03 Contents 4 15 2 Software Diagnostics and Calibration 4 14 5 Service 5 1 Laquid Eeaks eec Ree vue va e reges 5 1 5 2 Cleaning the Flow Cell
3. 5 2 5 3 Removing Trapped Air from the Flow Cell 5 2 5 4 Removing the Flow Cell 5 3 5 5 Replacing the Flow Cell Windows 5 4 5 6 Replacing the Flow Cell 5 5 527 Replacing the Deuterium 5 6 5 8 Replacing the Tungsten 5 9 5 9 Replacing the Main Power Fuses 5 11 A Specifications A 1 Physical b x Selene eee tk NUES ERES 1 2 Environmental 1 A3 Se E EE oa dI dd AO dc EE 1 AA Detector EE A 2 A 5 Flow Cells 5 eese ot eoe e E EEERS UP ences vn oe o Rs A 3 Heat Exchangers ccc sev HEEN EA 3 B Installation B 1 Facilities B 1 Doc 031644 02 9 03 iii PDA 100 Photodiode Array Detector B 2 Unpacking B 3 Installation B 3 1 B 3 2 B 3 3 B 3 4 B 3 5 B 3 6 hed Flow Cell Waste Line Detector Output Analog Relay TTL Control DX LAN Interface C Reordering Information Doc 031644 02 9 03 1 Introduction 1 4 Product Overview The PDA 100 Photodiode Array Detector is an optical detector capable of measuring the absorbance spectrum from 190 nm to 800 nm A deuterium lamp optimizes the UV range
4. 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 clean them with deionized water Refer to the pump user s manual for instructions Cleaning the pistons removes salt crystals that can abrade the piston thereby causing the main seal to wear out prematurely and allow leaks Replace the piston seals if there is a heavy salt build up on the pistons if the seals leak or if the pistons are replaced Refer to the pump user s manual for instructions Doc 031644 02 9 03 3 3 PDA 100 Photodiode Array Detector 3 2 Getting Started Before beginning operation of the PDA 100 check the following Press the Power switch on the front panel to turn on the detector see Figure 2 1 Make sure the Power LED is lighted but is not flashing If the Power LED is flashing the detector failed one of the electrical checks or optical checks performed during the power up sequence Turn on the appropriate lamp s in PeakNet 6 or Chromeleon if necessary The first time the detector power is turned on both lamps are on the factory default settings To change the default settings press F8 to display the Commands dialog box select UV to display UV related commands and then select UVLampPowerOnSetting and or VisLampPowerOnSett
5. EZ DIONEX PDA 100 PHOTODIODE ARRAY DETECTOR OPERATOR S MANUAL 2003 Dionex Corporation Now sold under the Thermo Scientific brand Thermo SCIENTIFIC Document No 031644 Revision 02 September 2003 2003 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 DX LAN PeakNet and Summit are trademarks or registered tr
6. Die Komponenten zum Z nden und Betreiben der Deuteriumlampe f hren Hochspannung Der Service darf nur von qualifiziertem Personal durchgef hrt werden WARNUNG Preamp Card The photodiode array is connected directly to the preamplifier The preamp gain is automatically adjusted to compensate for system variables such as lamp intensity Analog to digital conversion of the signal occurs on the Preamp card Preamp output is directed to the Data Processing card 2 8 Doc 031644 02 9 03 2 Description Data Processing Card The PDA 100 Moduleware resides on the Data Processing card Four BNC connectors on the card provide the analog recorder outputs Select the output scale polarity baseline offset and filter rise time from PeakNet 6 or Chromeleon In addition the Data Processing card provides the digital signal processing and conversion to log ratios when absorbance is measured Doc 031644 02 9 03 2 9 PDA 100 Photodiode Array Detector 2 5 Rear Panel Figure 2 5 illustrates the rear panel of the PDA 100 PDA 100 Serial Number I Fuse Holder e Main Power JUUUUUUUUUU JUUUUUUUUUUUUY Receptacle 2 96 sS Mm SEES ga LAN Identification LO Analog Outputs 7 J e j Number U Relay TTL DX LAN Drain Connectors Connector Tube Figure 2 5 PDA 100 Rear Panel Power Entry Th
7. Improving resolution 4 10 Stainless steel flow cell Chemical compatibility 2 6 3 15 A 3 B 3 Corrosion 3 15 Operating pressure A 3 Optical path length A 3 Part number 2 6 Volume A 3 Stainless steel systems Flow cell 2 6 Tubing connections 5 1 Step 3 15 Definition 3 24 Guidelines for selecting 3 24 Selection by software 3 24 System equilibration 4 3 T Technical Support at Dionex 4 1 5 1 Temperature ambient A 1 Reference mode selection 3 20 Timebase 4 3 Troubleshooting See also Diagnostics Baseline drift 4 6 Baseline noise 4 3 4 5 Diagnostic tests 4 14 DX LAN communication problem 4 2 4 10 Elution time is slow 4 3 Lamp does not light 4 7 PDA 100 does not respond 4 2 4 3 Peak shape is poor 4 12 Peak size is wrong 4 11 Spectra not collected 4 10 Spectral resolution is poor 4 10 Wavelength calibration fails 4 8 Wavelength verification fails 4 9 TTL control 2 12 Installation B 6 Pin assignments B 7 Tubing connections 3 2 5 1 Maintenance 3 29 Tungsten lamp 2 4 2 5 Calibration 4 8 Lamp does not light 4 7 Maintenance 3 30 Output waning 4 4 Part number 5 9 Power supply 2 8 Replacing 5 9 See also Lamps Time in use 5 10 Time to stabilize 3 4 4 3 4 6 Tungsten LED 2 2 Flashing 2 2 4 2 4 7 U UV wavelengths 2 5 V Ventilation 4 6 Visible focus lens 2 5 Visible wavelengths 2 5 W Warning icon 1 6 1 7 5 6
8. M Maintenance procedures 3 29 Mobile phases 3 2 Concentration guidelines 3 1 Degassing 3 1 4 4 Effect of pH on retention time 3 1 High background absorbance 4 8 Lamp stability after changing 4 3 4 6 Preparation 4 3 Reservoir material 3 2 Solvent quality 3 1 Doc 031644 02 9 03 Index 3 PDA 100 Photodiode Array Detector Temperature stabilization 2 6 Moduleware 2 9 4 14 Diagnostics 4 14 N Negative absorbance 3 8 3 15 Guidelines for selecting 3 26 Normal phase solvents 2 6 3 15 B 3 NOTES in manual 1 7 O Offset level 3 8 Operating parameters Optimization 3 15 3 22 3 24 3 26 Optical bench 2 3 Cooling 2 8 Leak sensor 2 3 Leak tray 2 3 Optical system Components 2 4 Illustration 2 4 P Parts replacement 5 1 C 1 See also Service procedures Use of non Dionex parts 5 1 Passivation 3 29 PDA 100 Photodiode Array Detector Applications 3 1 Automated control 3 5 3 8 3 9 Dimensions A 1 Installation instructions B 8 Maintenance 3 29 Parts replacement 5 1 Performance optimization 3 15 3 22 3 24 3 26 Power cord B 2 Power supply 2 7 A 1 B 2 Power switch B 2 Safety standards 1 6 Ship Kit B 1 B 4 Shutdown procedure 3 29 Spare parts C 1 Tubing connections 5 1 Unpacking instructions B 1 Warranty 5 1 Weight A 1 Peak height 3 16 3 19 Peak identification 1 2 1 3 3 18 Peak purity 1 2 1 3 3 5 3 18 Peak resolution 3 15
9. PeakNet 6 software 1 1 3D option 1 2 3 5 Control of PDA 100 3 5 3 8 3 9 Leak alarm 2 3 See also Chromatography software Peaks Asymmetrical 3 16 Co eluting 3 17 Improving height 4 11 Improving shape 4 12 PEEK flow cell Chemical compatibility 2 6 3 15 A 3 B 3 Operating pressure A 3 Optical path length A 3 Part number 2 6 See also Cells Volume A 3 PEEK systems Flow cell Tubing connections 5 1 PGM files 2 12 3 5 3 9 4 10 PGM Wizard 3 9 Photodiode array 1 1 2 4 2 5 2 8 Photodiode array detection 1 2 Advantages of 1 2 Polarity 2 9 Post column reagents 4 11 Degassing 4 4 Power cord 2 10 5 11 B 2 Power LED 2 2 Flashing 2 2 4 9 Index 4 Doc 031644 02 9 03 Index Power requirements A 1 Power supply 2 7 Power switch B 2 Power up diagnostic tests 2 2 4 14 Power up sequence fails 4 2 Preamp card 2 8 Preamp gain 2 8 Problems Contacting Dionex for help 4 1 5 1 See also Troubleshooting Pumping system requirements 3 2 R Rear panel Analog output connectors 2 12 Clearance required 4 6 B 1 DX LAN interface B 8 Fuses 2 11 Illustration 2 10 B 3 Power cord connection 2 10 Relay TTL connectors 2 12 Waste line 2 12 Recorder 4 11 B 5 Recorder outputs 2 9 Recorder range 3 8 Reference bandwidth 3 8 3 15 Definition 3 22 Guidelines for selecting 3 19 3 20 3 22 Reference intensity 3 20 Reference mode 3 8 Reference modes 3 20 Active reference
10. 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 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 Vis lamp connector and disconnect it from the 4 pin bulkhead 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 isopropyl alcohol IPA Doc 031644 02 9 03 5 9 PDA 100 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
11. 100 Serial Number Fuse Holder Main Power Receptacle D wv Relay TTL DX LAN Drain Connectors Connector Tube LAN Identification Number CHANNEL E AM kd f Analog Outputs Figure B 1 PDA 100 Rear Panel B 3 2 Flow Cell IMPORTANT Do not touch the cell windows If you touch a window clean it with denatured alcohol and a clean lens tissue IMPORTANT Do not use the PEEK flow cell with normal phase or chlorinated solvents these solvents will damage the cell Do not use the stainless steel flow cell with high pH salts the salts IMPORTANT Wee can cause corrosion contamination and metal leaching The flow cell 1s installed in the detector at the factory Follow the steps below to complete the cell installation 1 Grasp the PDA 100 front panel by the sides and pull straight off to remove 2 Connectthe cell inlet tubing to the union fitting on the heat exchanger tubing see Figure B 2 Doc 031644 02 9 03 B 3 PDA 100 Photodiode Array Detector 3 WIE Connect a backpressure line made from 0 25 mm 0 010 in ID tubing to the cell outlet connection see Figure B 2 The backpressure line should provide enough restriction to generate the small amount of backpressure 0 14 MPa to 0 34 MPa 20 psi 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 m
12. 190 nm to 380 nm and a tungsten lamp optimizes the visible range 380 nm 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 runs that do not require spectral data and it conserves disk space Key PDA 100 features include e Deuterium and tungsten lamps ensure low baseline noise high signal intensity and applications flexibility in the wavelength range from 190 nm to 800 nm e 1024 element photodiode array optimizes spectral resolution Abuilt in holmium oxide filter verifies wavelength calibration accuracy e 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 host computer running PeakNet 6 or Chromeleon software Release 6 1 or later The detector communicates with the host computer via the Dionex DX LAN interface Doc 031644 02 9 03 1 1 PDA 100 Photodiode Array Detector 1 2 To take full advantage of the capabilities of the PDA 100 order the 3D option for the software The 3D option is required in order to perform the following e 3D data presentation and spectral analysis real time or post run e Peak purity analysis with selectable criteria e Spectral libra
13. 3 2 The 3D control panel is available only when PeakNet 6 or Chromeleon includes the 3D software option Doc 031644 02 9 03 3 9 PDA 100 Photodiode Array Detector Creating a New PGM File 1 PeakNet 6 and Chromeleon contain a Program Wizard to facilitate the creation of new PGM files To activate the Wizard go to the File menu and select the New command A dialog box appears 2 Select Program File and click OK The initial Program Wizard screen is displayed Program Wizard Select Timebase Options The Program Wizard guides you through the creation of program files To start select the timebase where the program will run To skip the Program Wizard press Finish now Timebase a My Computer 5 ystem 1 PDA 100 Computer x mee 2 enm MELAB_1 C ADOS 7 Favorites Network Neighborhood Protocol My Computer D Enter connection information manually or pick a timebase from the list at right B A 3 Select the Timebase where the program will run 4 Click the Next button to continue 3 10 Doc 031644 02 9 03 3 Operation and Maintenance If the selected timebase includes other devices pump autosampler etc Program Wizard screens for these devices are displayed before the PDA 100 screens If necessary click the Next button in each screen for another device until the following screen is displayed Program Wizard Acquisition Options 5 Select the data Acquisition
14. 3 20 Inappropriate mode selected 4 6 See also Reference wavelength Turning off active reference 3 20 Reference wavelength 3 8 3 15 3 20 3 22 4 6 Definition 3 20 Guidelines for selecting 3 20 Inappropriate setting 4 4 Relay control 2 12 Installation B 6 Pin assignments B 7 Replacing parts 5 1 Use of non Dionex parts 5 1 Retention time 3 1 Rise time 2 9 3 15 Correlation with data collection rate 3 17 Definition 3 16 Effect on baseline noise 3 16 Guidelines for selecting 3 16 3 17 Inappropriate setting 4 5 Run LED 2 1 Flashing 2 3 S Safety icons 1 5 1 7 5 6 5 9 Safety messages 1 6 Salts 2 6 3 15 B 3 Sample bandwidth 3 15 Definition 3 19 Guidelines for selecting 3 19 Sample intensity 3 20 Sample rate See Data collection rate Sample wavelength Guidelines for selecting 3 18 Sensitivity 3 15 Separator column Backpressure increase 3 29 Service procedures Cell cleaning 5 2 Deuterium lamp replacement 5 6 Electronics components 5 1 Fuse replacement 5 11 Removing trapped air from cell 5 2 Tungsten lamp replacement 5 9 Ship Kit B 1 B 4 Shutdown procedure 3 29 Signal intensity 3 20 Slit optical 2 4 2 5 Software control 1 1 1 2 Source lens 2 4 2 5 Spare parts C 1 Doc 031644 02 9 03 Index 5 PDA 100 Photodiode Array Detector Spectra not collected 4 10 Spectral library 1 2 1 3 3 5 Spectrograph lens 2 4 2 5 Spectrum 2 4 2 5
15. 3 8 Average 3 15 Definition 3 25 Guidelines for selecting 3 25 B Backpressure B 4 Slow increase 3 29 Sudden increase 3 29 Index Backpressure line 4 4 B 4 Bandwidth 3 8 Setting is too narrow 4 5 Baseline drift 3 15 Reducing 3 20 Baseline noise 3 15 5 2 Causes 5 2 Reducing 3 16 3 19 3 20 3 22 4 12 Relationship to rise time 3 16 Baseline offset 2 9 Bolts 10 32 Part number B 4 Buffers 3 2 Bunch width 3 8 3 15 Guidelines for selecting 3 24 C Cable DX LAN Installation 4 2 4 3 4 10 B 8 Part number 4 2 4 3 4 10 B 8 Specifications B 8 Calculating absorbance 3 23 Calibration wavelength 3 8 4 15 Cards PC boards Data Processing card 2 9 Preamp card 2 8 Servicing 2 7 Cascading hubs B 8 Caution icon 1 6 1 7 5 6 5 9 Cells 2 5 2 6 3 15 Air bubble prevention 4 4 B 4 Air bubble removal 5 2 Backpressure line 4 4 B 4 Chemical compatibility 2 6 3 15 A 3 B 3 Cleaning procedure 2 6 5 2 B 3 Contaminants 4 4 Doc 031644 02 9 03 Index 1 PDA 100 Photodiode Array Detector Heat exchangers 2 6 Illustration 2 6 B 4 Leaks 2 3 Operating pressure A 3 Part numbers 2 6 Path length A 3 Volume A 3 Windows 2 5 2 6 B 3 Chlorinated solvents 2 6 3 15 B 3 Chromatography software Audit Trail 2 1 Error log 4 14 Optimizing PDA 100 performance 3 15 See also Chromeleon software See also PeakNet 6 software Chromeleon so
16. Detector 4 13 Poor Peak Shape Concentration of standard is too high column is overloaded Dilute the standard Install a sample loop with a smaller volume Concentration of standard is too low Increase the standard concentration Inappropriate mobile phase Do not use a mobile phase that absorbs strongly at the peak absorbance wavelength 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 refer to Section 3 4 Incorrect reference wavelength selected Select a different reference wavelength For guidelines to follow when selecting the reference wavelength refer to Section 3 4 Sample 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 also reduce peak height Reference bandwidth too wide Select a bandwidth that provides the resolution required to achieve the desired sensitivity A wider bandwidth reduces baseline noise but may increase the chance that the sample absorbs in the reference bandwidth thus causing reduced sensitivity and peak height 4 12 Doc 031644 02 9 03 de Troubleshooting 4 14 Error Message Not Enough Light to Perform Operation e Light signal is not reaching the
17. Detector detector again to verify that the problem has been resolved If the error message appears again contact Dionex Technical Support for assistance If you see a weak light or no light at all shining onto the business card the lamp intensity is too low Check that the flange of the 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 For lamp replacement instructions see Section 5 7 or Section 5 8 for the deuterium lamp or tungsten lamp respectively If the error message appears again contact Dionex Technical Support for assistance Blockage in cell Flush the cell with eluent 4 7 Wavelength Calibration Fails Flow cell contains air bubble or old mobile phase Flush mobile phase through the cell Cell not clear or mobile phase has high background absorbance Clean the cell as instructed in Section 5 2 If the detector fails the wavelength calibration again replace the flow cell windows see Section 5 5 Deuterium lamp may be defective If the Deuterium LED flashes or fails to light replace the deuterium lamp see Section 5 6 If the Deuterium LED is lighted but is not flashing run both the wavelength calibration and the wavelength verification from the Wellness panel see Section 4 15 2 If these fail remove the flow cell and repeat the wavelength calibration and the wavelength verification If the wavelengt
18. Flow Cells Cell Body PEEK or stainless steel Volume and PEEK cell 13 uL volume 10 mm 0 394 in path length Optical Path Stainless steel cell 13 uL volume 10 mm 0 394 in path length Length Maximum PEEK cell 2 MPa 300 psi Operating Stainless steel cell 3 MPa 500 psi Pressure Chemical e Do not use bases stronger than 0 1 M they will etch the Compatibility silica windows of the flow cells Do not use normal phase or chlorinated solvents with the PEEK flow cell they will damage the cell Do not use high pH salts with the stainless steel flow cell they will cause corrosion contamination and metal leaching A 6 Heat Exchangers NOTE Each flow cell assembly contains two built in heat exchangers see Section 2 3 1 Maximum PEEK cell 2 MPa 300 psi Operating Stainless steel cell 3 MPa 500 psi Pressure Volume PEEK cell 20 uL Stainless steel cell 9 uL Doc 031644 02 9 03 A 3 PDA 100 Photodiode Array Detector A 4 Doc 031644 02 9 03 B Installation B 1 Facilities Required Make sure the PDA 100 installation site meets the electrical and environmental specifications listed in Appendix A Install the PDA 100 on a sturdy workbench Allow at least 6 cm 2 4 in of clearance behind the PDA 100 for power connections and ventilation Do not block air flow to the detector during operation room air is inducted into the detector to cool the electronics and dissipate the heat generated by t
19. The power supply module contains connections to the AC mains and provides regulated low voltage power for the PDA 100 The power supply is rated at 130 W Power entry components are shielded and filtered to prevent electromagnetic interference EMT SHOCK AND FIRE HAZARD The power supply module operates at line potentials Refer all servicing to qualified personnel WARNING d alimentation lectrique fonctionne aux potentiels du secteur Faites DANGER D LECTROCUTION ET D INCENDIE Le module 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 Doc 031644 02 9 03 2 7 PDA 100 Photodiode Array Detector Lamp Power Supply The lamp power supply controls the deuterium and tungsten lamps it also supplies power to the variable speed fan that cools the optical bench NOTE The fan speed is controlled automatically Changes in fan speed may be audible especially when the lamp selection is changed or the ambient temperature fluctuates SHOCK HAZARD Components used to ignite and operate the deuterium lamp are at high potentials WARNING et faire fonctionner la lampe au deut rium sont a des potentiels DANGER D ELECTROCUTION Les composants utilis s pour allumer VAN lev s AVERTISSEMENT STROMSCHLAGGEFAHR
20. Time 6 Check or clear the 3DFIELD check box to indicate whether 3D data will be collected 7 Check or clear the check box for each 2D single wavelength channel to be collected 8 Click Next Doc 031644 02 9 03 3 11 PDA 100 Photodiode Array Detector The following screen is displayed Program Wizard UV Options 9 Select the Data Collection Rate and the Rise Time NOTE The PDA 100 performance can be optimized by careful selection of the data collection rate rise time and other operating parameters For details refer to Section 3 4 10 Select the Lamp status 11 Click Next 3 12 Doc 031644 02 9 03 3 Operation and Maintenance The following screen is displayed Program Wizard 3DFIELD Options Wavelength to 800 190 800 nm Reference Wavelength 750 190 800 nm Bandwidth 50 1 610 nm Finish Cancel Help 12 Select the sample Wavelength Reference Wavelength and Reference Bandwidth NOTE The Reference Wavelength plus one half the Reference Bandwidth cannot be outside the 3D Wavelength range If the values are outside this range the Reference Wavelength setting will default to the longest wavelength possible given the bandwidth In the screen shot above the selected parameters are acceptable because 750 nm plus 25 nm one half of 50 nm is less than 800 nm 13 Click Next Doc 031644 02 9 03 3 13 PDA 10
21. average of the data points between steps If you select a larger step size when the average parameter is off the selected rise time is valid but some data points will be skipped Average The average parameter operates in conjunction with the step parameter see Step When average is On PeakNet 6 or Chromeleon averages the data points between step intervals reports that value and noise is reduced NOTE The default setting for average On is recommended for most applications When average is Off PeakNet 6 or 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 size is more than double the rise time the system response will be 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 Doc 031644 02 9 03 3 25 PDA 100 Photodiode Array Detector Negative Absorbance NOTE The NegativeAbsorptionLevel command is available only if you are running PeakNet 6 40 SP3 or later or Chromeleon 6 50 SP1 or later and PDA 100 Moduleware version 2 0 or later Negative absorbance is the result of decreased absorption of the eluent after autozero which usually occurs at the beginning of a run Depending on certain buffer conditions this shift can result in flat baselines or truncated peaks if this occurs increase the NegativeAbsorp
22. back up and overflow inside the detector 2 12 Doc 031644 02 9 03 3 e Operation and Maintenance 3 1 Operating Guidelines 3 1 1 NOTE The PDA 100 Photodiode Array Detector is designed for use with IC ion chromatography BioLC and HPLC high performance liquid chromatography systems and should not be used for any other purpose If there is a question regarding appropriate usage 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 Mobile Phases Solvent quality significantly affects detection limits and instrument performance To ensure optimal performance of the PDA 100 follow the precautions below Strong bases can etch the silica windows of the flow cell If the mobile phase is a base make sure the mobile phase concentration does not exceed 0 1 M If the concentration of the base is greater than 50 mM disconnect the separator column and flush the system with deionized water for 5 minutes at 1 0 mL min immediately after the analysis 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 employs chemical supp
23. data processor Make sure that at least one lamp is turned on Low light throughput Remove the cell from the optical bench see Section 5 4 Insert a business card into the cell mounting location and check that bright light is shining onto the card If you can see bright light shining onto the business card remove the card from the optical bench run the lamp intensity calibration see Section 3 6 and then autozero the detector If no error message is displayed flush the cell with eluent and or clean the cell as instructed in see Section 5 2 Reinstall the cell in the optical bench and autozero the detector again to verify that the problem has been resolved If the error message appears again contact Dionex Technical Support for assistance If you see a weak light or no light at all shining onto the business card the lamp intensity 1s too low Check that the flange of the new 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 For lamp replacement instructions see Section 5 7 or Section 5 8 for the deuterium lamp or tungsten lamp respectively If the error message appears again contact Dionex Technical Support for assistance e Blockage or low light transmission in cell Flush the cell with eluent Doc 031644 02 9 03 4 13 PDA 100 Photodiode Array Detector 4 15 Diagnostics 4 15 1 4 15 2 Moduleware Run Ti
24. discussed in this section Operating Parameter Flow cell material Rise time Data collection rate Sample wavelength Sample bandwidth Reference wavelength Reference bandwidth Step Bunch width 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 Baseline noise rise time data collection rate disk space Spectral resolution peak match disk space Rise time data collection rate Peak detection baseline noise linearity Set automatically by PeakNet 6 or Chromeleon Flow Cell Material The flow cell material must be chemically compatible with the mobile phases and analytes of interest Do not use the PEEK flow cell P N 056346 with normal phase or chlorinated solvents these solvents will damage the cell Do not use the stainless steel flow cell P N 056126 with high pH salts this may result in corrosion contamination and metal leaching Doc 031644 02 9 03 3 15 PDA 100 Photodiode Array Detector Rise Time Rise time is a measure of how quickly the PDA 100 responds to a change in signal The rise time can be set to 0 1 0 2 0 5 1 0 2 0 default or 5 0 seconds The selected rise time is applied to all data collected and to both analog and digital output Select a rise time that i
25. 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 Section 3 4 for more information 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 The filter paddle is tested during the autozero routine If the software displays an error message that the filter paddle test failed remove the flow cell check that at least one lamp is on and then autozero the detector If the error message appears again contact Dionex Technical Support for assistance Doc 031644 02 9 03 4 5 PDA 100 Photodiode Array Detector 4 4 Drifting Baseline Fluctuations in ambient temperature Make sure the PDA 100 installation site temperature remains consistent Allow at least 6 cm 2 4 in 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 3 Check that solvent flow is directed to the cell inlet and out the cell outlet Select a reference wavelength see Section 3 4 New lamp not burned in After installing a new lamp allow from 8 to 24 hours for the lamp to stabilize Lamp cover flow cell cover or front panel is missing Do not operate the PDA 100 unless the lamp cover fl
26. in the manual and the safety labels on the detector Describes the PDA 100 front panel LED indicators inside front panel optical system and rear panel connections Presents an overview of PDA 100 operation as well as guidelines for optimizing detector performance Lists routine preventive maintenance procedures Lists problems that may occur along with step by step instructions for resolving them Contains step by step instructions for routine service and parts replacement procedures Lists the PDA 100 specifications and installation site requirements Describes how to install the PDA 100 including the DX LAN connections to the host computer running Dionex chromatography software Lists spare parts for the detector Doc 031644 02 9 03 PDA 100 Photodiode Array Detector 1 3 1 Safety Messages and Notes 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 gt DANGER Indicates a potentially hazardous situation which if not avoided may result in death or serious injury gt WARNING Indicates a potentially hazardous situation which if not avoided may result in minor or moderate injury gt CAUTION Indicates t
27. outputs four analog signals at all times even when not interfaced to a computer Data is presented at the analog output channels whenever the detector power is on Use a chart recorder or other voltage measuring device to monitor the channels When the PDA 100 power is first turned on the analog output settings are at the factory defaults see the table below Channel Single Sample Reference Full Scale Offset Wavelength Bandwidth Wavelength Output 210 4 Off 1 0 AU 10 254 4 Off 1 0 AU 10 272 4 Off 1 0 AU 10 520 10 Off 1 0 AU 10 These factory default settings are also in effect Rise time 2 0 seconds e Lamp status The deuterium and tungsten lamps are on Stand Alone Operation The table below lists the TTL inputs and the PDA 100 parameters they control during stand alone operation TTL Input PDA 100 Parameter TTL lin Autozero TTL2in Remote inject TTL 3 in Deuterium lamp on off TTL4in Tungsten lamp on off 3 28 Doc 031644 02 9 03 3 Operation and Maintenance 3 6 Routine Maintenance The following maintenance procedures may be performed by the user Other maintenance procedures must be performed by trained Dionex Service 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 continuous flow at 0 2 mL min This rinses corrosive acids salts or bases from the flow paths Periodi
28. 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 031644 02 9 03 5 e Service 5 4 Removing the Flow Cell Remove the flow cell from the optical bench prior to inspecting the cell for leaks or obstructions replacing the cell windows see Section 5 5 or installing a new cell see Section 5 6 1 Grasp the detector 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 Remove the flow cell cover from the inside front panel Remove the tubing bracket from the lamp cover Nn WwW Optical Bench Guide for Lamp Wires Flow Cell gt Lamp Wires SA Deuterium Lamp Flow Cell Cover 4 E SY VA 5 S D Bracket K A v Flow Cell Outlet Tubing Remove the flow cell inlet tubing from the tubing guide in the lamp cover Squeeze the handle of the flow cell and pull it out of the optical bench Figure 5 1 Removing the Flow Cell Doc 031644 02 9 03 5 3 PDA 100 Photodiode Array Detector 5 5 Replacing the Flow Cell Windows Contaminated flow cell windows can s
29. 0 Photodiode Array Detector The following screen is displayed Program Wizard UV Channels Options Channel Wavelength Bandwidth RefWavelength 10 Off RefBandwidth Recorder Range 50 f i e I 10 ort 50 1 0000 10 Off 50 1 0000 10 on an 10000 M E RR REGERE J 10 750 50 1 lt L Frin Cancel Help 14 Program the single wavelength channels by selecting the Wavelength Bandwidth Reference Wavelength and Reference Bandwidth for each channel NOTE The settings selected for UV VIS 1 through UV VIS 4 apply to both analog outputs and digital outputs UV channel 1 analog output 1 UV2 analog output 2 etc Specify the Recorder Range in mAU per volt for each analog output that will be collected NOTE When the Reference Wavelength is Off the Reference Bandwidth is not used and the sample wavelength and sample bandwidth are used as reference parameters 15 After selecting all PGM file parameters click Finish 3 14 Doc 031644 02 9 03 3 Operation and Maintenance 3 4 Optimizing Detector Performance The performance of the PDA 100 can be optimized by careful selection of the operating parameters Section 3 4 defines several operating parameters describes how they interact with each other offers guidelines for selecting them and includes example chromatograms The following table summarizes the topics
30. 5 9 Warranty voiding 5 1 Waste line 2 12 Installation B 5 Wavelength 3 8 Wavelength calibration 1 1 3 8 4 9 4 15 Wavelength verification 2 5 4 9 Wavelengths single 1 1 3 18 Reference modes 3 20 Index 6 Doc 031644 02 9 03
31. AU min Figure 3 5 Effect of Reference Wavelength on Baseline Drift Doc 031644 02 9 03 3 21 PDA 100 Photodiode Array Detector Reference Bandwidth The reference bandwidth which is analogous to the conventional bandwidth of a channel serves to average several diode signals of the reference wavelength A reference bandwidth is required only when a reference wavelength active mode is selected When the reference wavelength is off the reference bandwidth is the same as the sample bandwidth Select a reference bandwidth in an area of the spectrum where the sample does not absorb The reference bandwidth should be 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 3 22 Doc 031644 02 9 03 3 Operation and Maintenance Example Chromatogram Selecting the Sample Wavelength Reference Wavelength and Reference Bandwidth Figure 3 6 shows the spectrum of caffeine The operating conditions are Sample wavelength 272 nm Sample bandwidth 5 nm Reference wavelength 325 nm Reference bandwidth 51 nm These settings calculate the absorbance by the following equation avg 300 to 350 AUE 7 0210 to 274 offset at autozero mAU amp Sample Bandwidth 5 nm 270 nm to 274 nm A 4 Reference Bandwidth 51 n
32. Hz the software sets the step to 0 2 second The following table indicates the automatically selected step setting for each data collection rate 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 3 24 Doc 031644 02 9 03 3 Operation and Maintenance Step Override IMPORTANT Selecting an inappropriate step setting may cause loss of sensitivity skipped data points and other problems Guidelines for overriding the automatic selected step setting are provided for reference by advanced users only In almost all cases the step setting selected by PeakNet 6 or Chromeleon is preferred However it is possible to override this setting by manually changing the step in the PGM file or the control panel For example it may be desirable 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 Step 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 5096 If you select a larger step size when the average parameter is on see Average the system response is a combination of the selected rise time and the
33. N 960281 must be connected between the Ethernet hub P N 056909 and the DX LAN connector on the host computer s internal DX LAN interface card IMPORTANT When using 10BASE T cabling always install an Ethernet hub If you simply plug the 10BASE T cable from the PDA 100 into the connector on the host computer s DX LAN card the connection will not work Detector and or control panel not connected to timebase Add the PDA 100 control panel to a software timebase 4 3 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 connections are made with Dionex ferrule fittings refer to Installation of Dionex Ferrule Fittings for tightening requirements 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 If the noise is synchronized with the pump s
34. On Off toolbar button to stop manual data acquisition after the desired run time 9 Data collected during the run may be saved to a sequence To retrieve the data select the assigned sample name within the sequence Serial Numbers Acquisition On Off PeakNet Autosampler Pump PDA Timebase System_1 Computer name MELAB 1 Edt View Workspace Qualification Control Batch Window Help laj xl eMas BEER ne las ER NN NN S o E31 Sample Datasource PDA_AUTOSAMPLER_PUMP_0 Elapsed Time 121 308 Audit Trail 11 17 57 0 000 UV VIS 3 AcqOn FI 11 17 57 0 000 UV VIS 4 AcqOn 11 17 57 0 000 UV VIS 5 AcqOn 13 19 15 121 308 StopFlow PDA 100 Detector LMC om Setup Parameters 254 EIg 1 280 aL Off EI UV 1 0 1681 MAU UV 2 0 1037 mau Autozero 0 228 Detector Signals for UV1 and UV2 Wavelengths Pump Pressure Chromatogram s Limits 70 min 0 02 mAU PKEENAN System_1 Stopped Figure 3 1 PDA 100 2D Control Panel Example 3 6 Doc 031644 02 9 03 3 Operation and Maintenance Acquisition On Off lt H ang response on ASI O0 infectStite 1246 56 0 000 Sampler ot inject response 13 46 56 0 000 3CFIELD caon 15 46 54 0 000 UV MS en 12 30FIELD Aeg OT
35. Photodiode Array Detector 5 7 Replacing the Deuterium Lamp 1 Stop the PeakNet 6 or 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 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 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 c
36. RefWavelength is Off the RefBandwidth setting has no effect Sets the sample wavelength up to five sample wavelengths can be programmed Sets the bandwidth of the sample wavelength Bunching or averaging the signals of adjacent wavelengths reduces the size of the 3D data stored Adjusts the negative absorbance this permits peaks to be seen even when the eluent decreases absorbance Runs the wavelength calibration procedure 3 8 Doc 031644 02 9 03 3 Operation and Maintenance 3 3 2 Programmed Control A PGM file is a list of time precise control commands created by the user for automated operation of the PDA 100 The user can create PGM files automatically with the help of the PGM Wizard or manually by editing an existing PGM file NOTE This section provides a brief overview of detector control For complete operating instructions refer to the PeakNet 6 or Chromeleon online Help or user s manual Summary of programmed control 1 Start PeakNet 6 or Chromeleon 2 Create anew PGM file see the following section or modify an existing program 3 Create a new sequence or modify an existing sequence 4 Select one of the PDA 100 default control panels e DIONEX PUMP PDA AUTOSAMPLER PAN the 2D control panel monitors chromatograms of up to five signals see Figure 3 1 e DIONEX PUMP PDA3D AUTOSAMPLER PAN the 3D control panel monitors chromatograms contour plots and spectra on line see Figure
37. Relay and TTL connections see Figure B 3 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 screwdriver RELAY OUT TTL TTLIN TTL OUT GND 1 2 12 12 3 4 1 2 12 34 5 6 7 8 9 10 1112 Figure B 3 Relay and TTL Connector Doc 031644 02 9 03 B Installation The table below describes the pin assignments for the Relay and TTL connectors Connections 1 and 2 can be configured in the software to switch any low voltage control The switched current must be less than 200 mA and 42 V peak Pin Assignment 1 Relay 1 output 2 Relay 1 output 3 Relay 2 output 4 Relay 2 output 5 TTL 1 output 6 TTL 2 output 7 TTL 1 input 8 TTL 2 input 9 TTL 3 input 10 TTL 4 input 11 input or output 12 input or output Input Pin Function Active Ground Active Ground Active Active Active Autozero Active Remote inject Active UV lamp on off Active Visible lamp on off Ground 1 Ground 2 Doc 031644 02 9 03 B 7 PDA 100 Photodiode Array Detector B 3 6 DX LAN Interface In order to communicate with a host computer running Dionex software the DX LAN interface must be installed Connect an unshielded twisted pair DX LAN cable P N 960281 from the RJ 45 LOBASE T connector on the PDA 100 rear panel to a combo IOBASE T Ethernet hub P N 056909 Install
38. Serial Numbers Detector Signals for UV1 and UV2 Wavelengths Figure 3 2 PDA 100 3D Control Panel Example Doc 031644 02 9 03 3 7 PDA 100 Photodiode Array Detector PeakNet 6 and Chromeleon include several detector commands These commands are selected from the default control panel or the Commands dialog box selected from the Control menu or by pressing F8 The table below lists several of the most frequently used detector commands For more information refer to the online Help PDA 100 Command Connect UV Lamp On Off Vis Lamp On Off UVLampPowerOnSetting VisLampPowerOnSetting Autozero Recorder_Range Offset_Level Reference_ Mode RefWavelength RefBandwidth Wavelength Bandwidth Bunch Width NegativeAbsorptionLevel WavelengthCal Function Indicates whether the PDA 100 is connected to the server and the selected timebase Turns the deuterium lamp on and off Turns the tungsten lamp on and off Selects the power up setting for the deuterium lamp Selects the power up setting for the tungsten lamp Adjusts the output to zero Sets the full scale recorder output range Sets the offset applied to the recorder output Reports the reference mode Sets the reference wavelength If RefWavelength is Off the reference value is the first data point of the sample wavelength and bandwidth after autozero is performed Sets the bandwidth of the reference wavelength if one is selected If
39. ademarks of Dionex Corporation Teflon and Tefzel are registered trademarks of E I duPont de Nemours amp Company PRINTING HISTORY Revision 01 May 2000 Revision 02 September 2003 Contents 1 Introduction 1 1 1 2 1 3 1 4 Product Overview veces poer ese pex big Gah e peni pues 1 1 Theory of Photodiode Array Detection 1 2 1 2 1 Advantages of Photodiode Array Detection 1 2 About This Manual 1 5 1 3 1 Safety Messages and Notes 1 6 Satety Eabels craw sens eae uke CITUR RE wile RE ed 1 8 2 Description 2 1 2 2 2 3 2 4 2 5 Front Panel 1x4 Rods ee Ide LR edd AAS Sada Maoh den 2 1 Inside Front Panel onenig eaea a ot pter epus eme EU RR Ec 2 3 Optical Systems gn Rp EP pa er e eR RR Rd 2 4 2 3 1 rt etre ten ees e edes em eue 2 6 Flectronies c RH ERU pe eR RA E NUR 2 7 Rear Panel 2 we gelesene dle de Lr OR TES 2 10 3 Operation and Maintenance 3 1 3 2 Operating Guidelines 0 0 eee eee 3 1 S Mobile PRASGS teg yea ars ey n E Pao 3 1 3 1 2 Solvent Delivery System 3 2 Getting Started i os seed Ene Oe OH d ue MAR EAS 3 4 Doc 031644 02 9 03 PDA 100 Photodiode Array Detector 3 3 3 4 3 5 3 6 Routine 3 5 3 33 Panell Controls 2s 3 5 3 3 2 Programmed
40. 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 2 07 MPa 300 psi Check for leaks around the windows If there is any leakage tighten the window nut s with the windows replacement tool until the leak stops Dry the cell thoroughly with a lint free optical grade tissue 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 silica windows and you do not want to replace them see Section 5 5 1 2 Remove the flow cell from the optical bench see Section 5 4 Squeeze the handle of the new flow cell PEEK P N 056346 stainless steel P N 056126 and insert it straight into the optical bench Release the handle and then pull it forward slightly If there is a click the cell is properly mounted If there is no click rotate the handle slightly just until the cell clicks into place Thread the flow cell inlet tubing through the tubing guide on the lamp cover and reinstall the tubing bracket see Figure 5 1 Thread the flow cell outlet tubing through the slot on the side of the flow cell cover Replace the cover and reconnect the cell inlet and outlet tubing Push the detector front panel into place Doc 031644 02 9 03 5 5 PDA 100
41. aptive in the lamp base and do not need to be removed 10 Inspect the new deuterium lamp P N 9390167 for fingerprints and dust If necessary clean the lamp with isopropyl alcohol IPA 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 5 6 Doc 031644 02 9 03 5 e Service 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 15 Thread the flow cell inlet tubing through the tubing guide on the lamp cover and reinstall the tubing bracket Flow Cell A Cover Deuterium Screw Ire Gui Lamp sE Wire Guide UV Lamp Connector 6 pin Bulkhead Connector D 4 Bulkhead Connector Locating Tungsten Visible Lamp Connector Pin Red Power Lead Lamp Le Sensor Figure 5 3 Lamp C
42. ate concentrations of acetonitrile etc are acceptable for a PEEK system Other solvents and high concentrations of acetonitrile require a stainless steel system All tubing connections should be Teflon Tefzel PEEK stainless steel or titanium as required for the 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 3 2 Doc 031644 02 9 03 3 Operation and Maintenance 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 gloves 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 Remove the column and suppressor if installed 2 Connect the line exiting the injection valve directly to the flow cell 3 Flush the system with deionized water at 1 0 mL min for 20 minutes 4 Flush the system with methanol at 1 0 mL min for 20 minutes For very sensitive applications continue flushing for several hours
43. cally check the drain tube connected to the leak tray in the bottom of the optical bench verify that the tubing is unclogged and remains routed below the leak tray Periodically check the flow cell tubing connections for leaks or restrictions Replace tubing and fittings as necessary 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 slow 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 However if the backpressure remains high remove the fittings and tubing from part of the flow path section by section start at the waste line and work back upstream until the section causing the substantial backpressure is identified Replace tubing and fittings as necessary Periodically repassivate stainless steel systems This is especially important when operating with extremes of pH which shortens the life of the passivation finish or after a major disassembly For instructions see Passivation of Stainless Steel Systems and Component
44. d water or methanol through the system during the wavelength verification test Doc 031644 02 9 03 4 9 PDA 100 Photodiode Array Detector 4 9 Faulty DX LAN Communication PDA 100 not detected on DX LAN When the host computer is powered up PeakNet 6 or Chromeleon scans the DX LAN for all installed instruments If the PDA 100 power is off the detector cannot be identified Before turning on the computer power make sure the detector power is turned on DX LAN interface incorrectly installed Check the following for installation instructions see Section B 3 6 e A 10BASE T DX LAN cable P N 960281 must be connected between the DX LAN connector on the PDA 100 rear panel and the Ethernet hub P N 056909 e A 10BASE T DX LAN cable P N 960281 must be connected between the Ethernet hub P N 056909 and the DX LAN connector on the host computer s internal DX LAN interface card IMPORTANT When using 10BASE T cabling always install an Ethernet hub If you simply plug the 10BASE T cable from the PDA 100 into the connector on the host computer s DX LAN card the connection will not work 4 10 No Spectra Collected Spectral range was not programmed Select a spectral range in the PGM file or control panel Detector and PGM file or control panel connected to different timebases Add the PDA 100 to the same timebase as the PGM file or control panel 4 11 Low Spectral Resolution Bunch width too wide Select a bunch
45. e drain tube is above the drain port the drip tray may overflow inside the detector Detector Output Analog The PDA 100 provides four analog outputs controlled by absorbance wavelengths 1 through 4 in PeakNet 6 or Chromeleon software They provide a 1 volt output maximum The software controls the full scale absorbance output and offset within the 0 to 1 volt range Connect a recorder or an integrator to the ANALOG OUT connector on the PDA 100 rear panel see Figure B 1 Doc 031644 02 9 03 B 5 PDA 100 Photodiode Array Detector B 3 5 gt CAUTION gt WARNING gt AVERTISSEMENT gt WARNUNG Relay TTL Control 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 card SHOCK AND FIRE HAZARD Inputs and outputs are not rated for connection to an AC power main DO NOT CONNECT TO 100 115 220 230 OR 240 VAC POWER SOURCES FIRE OR ELECTROCUTION MAY RESULT DANGER D ELECTROCUTION D INCENDIE Le module d alimentation lectrique fonctionne aux potentiels du secteur Faites effectuer toutes les r parations par un personnel qualifi STROMSCHLAG UND BRANDGEFAHR Das Modul zur Stromversorgung wird mit Netzspannung betrieben Der Service darf nur von qualifiziertem Personal durchgef hrt werden The PDA 100 Ship Kit includes a 12 pin connector for
46. e for sample absorbance The cell has a flat window on each side 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 measures a narrow band of the spectrum A spectrum is obtained by measuring the light intensity of each wavelength and reporting the range of results Doc 031644 02 9 03 2 5 PDA 100 Photodiode Array Detector 2 3 1 Flow Cell The PDA 100 flow cell assembly see Figure 2 4 is available in PEEK or 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 53 E Cell Outlet Tubing Cell Inlet Tubing md rl j Flow Cell 7 Heat Exchangers P d Spring Clip Figure 2 4 Flow Cell Assembly Flow Cell Cell Path Le
47. e power entry is socketed for a modular power cord IEC 320 C13 The PDA 100 operates from input voltages over a range from 85 Vac to 264 Vac 47 Hz to 63 Hz power and requires a grounded single phase power source The input power is 162 W maximum and the output power is 130 W maximum 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 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 2 10 Doc 031644 02 9 03 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 bz
48. e wavelength active reference mode for gradient analyses and turning off the reference wavelength for isocratic analyses in a laboratory with a stable ambient temperature For more information see Section 3 4 4 5 Lamp Does Not Light or Lamp LED Is Flashing 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 The average lamp lifetime is 1000 hours although lamps often last longer with only minimal deterioration in performance 4 6 Deuterium Lamp Intensity Count Too Low If the deuterium lamp intensity reading is low see Section 3 6 follow these steps to resolve the problem Light signal is not reaching the data processor reading is lt 1000 counts Make sure that at least one lamp is turned on Low light throughput reading is 10 000 000 counts Remove the cell from the optical bench see Section 5 4 Insert a business card into the cell mounting location and check that bright light is shining onto the card If you can see bright light shining onto the business card remove the card from the optical bench run the lamp intensity calibration see Section 3 6 and then autozero the detector If no error message is displayed flush the cell with eluent and or clean the cell as instructed in see Section 5 2 Reinstall the cell in the optical bench and autozero the Doc 031644 02 9 03 4 7 PDA 100 Photodiode Array
49. ee Section 3 5 or the settings selected the last time the detector was controlled by the host 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 3 2 or controlled manually through a control panel in the software The Relay outputs can be programmed to switch any low voltage control The switched current must be less than 200 mA and 42 V peak For installation instructions for the Relay and TTL connectors refer to Section B 3 5 DX LAN Connector The 1OBASE T DX LAN RJ 45 connector on the rear panel allows communication between the PDA 100 and the host computer running PeakNet 6 or Chromeleon software The PDA 100 is usually connected directly to the computer using a IOBASE T DX LAN cable P N 960281 For installation instructions refer to Section B 3 6 Waste Line Waste exits the detector via the drain tube connected to the rear panel The drain tube must be routed downward below the leak tray Check periodically to verify that the drain tube is not clogged or bowed upward and that the tubing remains routed below the leak tray For installation instructions see Section B 3 3 IMPORTANT The drain tube must remain routed below the drain port If the drain tube is above the drain port the drip tray may
50. elength 254 nm Reference wavelength Off Flowing water at 1 0 mL min 10 35 MPa 1500 psi EEN Itten WCS m Sample Bandwidth 8 vi Noise 14 AU Sample Bandwidth 4 Noise 16 LAU 002041 0 03004 _ Sample Bandwidth 1 Noise 26 AU 0 04004 0 0500 Figure 3 4 Effect of Sample Bandwidth on Baseline Noise Doc 031644 02 9 03 3 19 PDA 100 Photodiode Array Detector 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 and off To select the active reference mode enter a wavelength within the scanning ability of the PDA 100 The selected wavelength will be used as the reference wavelength The reference intensity will vary over time as 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 both wavelengths are within the UV spectrum of the deuterium lamp 190 nm to 380 nm Active reference mode minimizes baseline drift and is ideal for gradient analyses where the basel
51. escribes the operating problem there possible causes of the problem are listed in order of probability along with the recommended courses of action 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 4 1 Flashing LED Run LED is flashing An alarm was activated Check the software Audit Trail for an error message Deuterium LED is flashing The lamp did not power on properly Check the software Audit Trail for an 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 Technical Support for assistance Tungsten LED is flashing The lamp did not power on properly Check the software Audit Trail for an error message If necessary replace the lamp see Section 5 8 Power LED is flashing The detector failed one of the checks performed during the power up sequence see Section 4 15 1 or the wavelength calibration check that is performed the first time the deuterium lamp is turned on after power up Check the software Audit Trail for an error message Doc 031644 02 9 03 4 1 PDA 100 Photodiode Array Detector 4 2 No Detector Response Detector power not turned on Check that the main power switch is turned on Check that the power cord is connected from the rear panel to a
52. ftware 1 1 1 2 3D option 1 2 3 5 Control of PDA 100 3 5 3 8 3 9 Leak alarm 2 3 See also Chromatography software Components elute slowly 4 3 Control panel 2 12 3 5 Selecting parameters 3 5 D Danger icon 1 6 1 7 5 6 5 9 Dark signal 2 5 Data collection rate 3 15 Correlation with rise time 3 17 Definition 3 17 Guidelines for selecting 3 17 Relationship to step 3 24 Data files occupy too much disk space 3 17 Data points 3 17 3 24 Minimum number per peak 3 17 Data Processing card 2 9 Analog output connectors 2 9 Lithium battery disposal 5 1 Deuterium lamp 2 4 2 5 Calibration 4 8 Lamp does not light 4 7 Maintenance 3 30 Output waning 4 4 Part number 5 6 Power supply 2 8 Replacing 5 6 See also Lamps Time in use 5 8 Time to stabilize 3 4 4 3 4 6 Deuterium LED 2 1 Flashing 2 1 4 2 4 7 Diagnostic tests 4 14 Power up 2 2 4 14 Run time testing 4 14 Dionex Technical Support 4 1 5 1 Disk space 3 15 3 17 3 18 Conserving 1 1 3 18 Drain tube 2 12 B 5 DX LAN connector 2 12 DX LAN interface 1 1 Cable specifications B 8 Communication problem 4 2 4 10 Installation 4 2 4 10 B 8 E Electrical specifications A 1 Electromagnetic interference EMI 2 7 Electronics 2 7 Repair 2 7 5 1 Electrostatic discharge ESD 2 7 Equilibration system 4 3 Error log in software 4 14 Errors See Troubleshooting F Fan 2 8 Speed 2 8 Ferr
53. h calibration still fails contact Dionex Technical Support for assistance Doc 031644 02 9 03 de Troubleshooting 4 8 Wavelength Verification Fails Detector wavelength requires recalibration In PeakNet 6 or Chromeleon select the UV Calibration command on the Wellness panel Or press F8 to display the Commands dialog box and select UV to display UV related commands Select the UV_Calibration command and then select WavelengthCal 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 briefly Turn on the power again and verify that the Power LED is lighted but is not flashing If solvent sits in the cell for an extended period it decreases the intensity of the light passing through the cell To ensure reliable data maintain a constant flow through the cell Flushing the cell with deionized water or methanol each time the detector is powered up is helpful Lamp is dimming Check the lamps as follows In PeakNet 6 or Chromeleon press F8 to display the Commands dialog box and select UV to display UV related commands Select UVLampAge and then VisLampAge If either lamp has been in operation for more than 1000 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 deionize
54. hat the function or process of the instrument may be IMPORTANT impaired Operation does not constitute a hazard 1 6 Doc 031644 02 9 03 1 Introduction gt DANGER gt AVERTISSEMENT gt MISE EN GARDE gt ACHTUNG gt WARNUNG gt VORSICHT Messages d avertissement en frangais Signale une situation de danger imm diat qui si elle n est pas vit e entrainera des blessures graves a mortelles Signale une situation de danger potentiel qui si elle n est pas vit e pourrait entrainer des blessures graves mortelles Signale une situation 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 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 Sch den 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 a
55. he 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 flow cell cover and lamp cover are in place Optical detectors are sensitive to vibrations Make sure the PDA 100 installation site is vibration free B 2 Unpacking Carefully remove the PDA 100 from the shipping container IMPORTANT Lift the PDA 100 by the side or bottom only the front panel snaps into place and must not be used for lifting the detector Do not turn on the PDA 100 unless it is at room temperature 10 C to 40 C 50 F to 104 F If the detector is moved from a cold environment to a warm environment wait at least 1 hour for condensation to evaporate before turning on the mains power The PDA 100 Ship Kit contains the parts required to install the detector Product Line PDA 100 Flow Cell Material Ship Kit DX 600 P N 057061 PEEK P N 056471 BioLC P N 054105 PEEK P N 056471 Summit P N 054100 Stainless Steel P N 054103 Doc 031644 02 9 03 B 1 PDA 100 Photodiode Array Detector Installation B 3 1 Power 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 gt WARNING The power supply cord is used as the main disconnect device Make sure the socket outlet is located nea
56. ignificantly increase baseline noise and cause wavelength calibration to fail If cleaning the cell see Section 5 4 does not eliminate these problems replace the two silica flow cell windows The flow cell windows replacement kit P N 060498 contains all of the parts required for this procedure 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 it on a clean work surface 2 Put ona pair of latex gloves 3 Using the windows replacement tool P N 060497 remove one of the window nuts from the flow cell see Figure 5 2 It does not matter which window nut you remove first 4 Remove and discard the old window NNE Cell Outlet Tubing 4 e Cell Inlet Tubing O Ring Groove SYN CA d gt O Ring P N 054136 Window P N 054135 Window Nut Figure 5 2 Replacing the Flow Cell Windows Light inlet side shown Doc 031644 02 9 03 5 e Service 5 Use tweezers to carefully remove the O ring from the groove see Figure 5 2 Do not scratch the groove IMPORTANT Scratches in the groove will prevent the new O ring from sealing properly and will cause leaks 10 11 Install a new O ring P N 054136 in the groove Place a new window P N 054135 into the counterbore in the window nut Screw the window into place Using the windows replacement tool tighten the window nut until snug and then turn
57. ine may shift Active mode also helps compensate for fluctuations in ambient temperature caused by air conditioning NOTE When active reference mode is selected be sure to select a reference wavelength and reference bandwidth in a quiet area of the spectrum where little absorption occurs To deselect the active reference mode enter Off as the reference wavelength The intensity reading at the time of autozero will be used as the reference wavelength Operating when the reference wavelength is off ensures the lowest baseline noise when running an isocratic analysis in a laboratory with stable ambient temperature It also ensures that fluctuations in the reference intensity do not cause additional noise 3 20 Doc 031644 02 9 03 3 Operation and Maintenance Example Chromatogram Selecting the Reference Wavelength Figure 3 5 shows results obtained from two different channels within the same run When the reference wavelength 1s turned off baseline drift is 120 pAU hour when a reference wavelength active mode is selected baseline drift is reduced to 40 pAU hour The operating conditions are Sample wavelength 520 nm Sample bandwidth 10 nm Reference bandwidth 50 nm active reference mode only Flowing water at 1 0 mL min 10 35 MPa 1500 psi Reference Wavelength Mode Off Baseline Drift 120 AU hour mAU min Reference Wavelength Mode Active Baseline Drift 40 AU hour m
58. ing The first time the deuterium lamp is turned on the detector checks the wavelength to pixel assignment if a problem is detected the Power LED will flash If this occurs flush the flow cell with deionized water or methanol and then turn off the detector power briefly Turn on the power again and verify that the Power LED is lighted but is not flashing NOTE If solvent remains in the flow cell for an extended period it may form a bubble or decrease the intensity of the light passing through the cell This will cause the detector to fail the wavelength calibration check performed the first time the deuterium lamp is turned on after power up and or the autozero Make sure the Deuterium and or Tungsten LEDs on the detector front panel are lighted see Figure 2 1 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 3 4 Doc 031644 02 9 03 3 Operation and Maintenance 3 3 Routine Operation During routine operation the PDA 100 is controlled from a host computer running either PeakNet 6 or Chromeleon software The following sections describe the two modes of software control panel control in which commands are executed directly from a control panel and automated control control from a PGM file NOTE The 3D software opti
59. ing the DX LAN Cable 1 Install the combo I0BASE T Ethernet hub P N 056909 on a workbench or on the wall For installation instructions and site requirements refer to the installation guide shipped with the hub 2 Plug the IOBASE T DX LAN cable P N 960281 into a TOBASE T port on the front panel of the hub The 10BASE T DX LAN cable is a Category 5 unshielded twisted pair cable Do not substitute a cable of an inferior grade Failure to use the correct cable will cause the PDA 100 to lose communication with the host computer 3 Connect the other end of the cable into the 1OBASE T DX LAN connector on the PDA 100 rear panel see Figure B 1 4 Connect a IOBASE T cable P N 960281 from a 1OBASE T port on the hub to the IOBASE T port on the host computer s internal DX LAN card If the connection is via port 8 on the hub set the Normal Uplink push button to Normal NOTE Installation instructions for the host computer s internal DX LAN card are in Installing the Dionex PeakNet 6 System Document No 031631 When using 10BASE T cabling always install an Ethernet hub If you simply plug the 10BASE T cable from the PDA 100 into the connector on the host computer s DX LAN card the connection will not work Cascading Hubs Cascading or connecting hubs together through their 1OBASE T ports increases the number of ports or the number of users supported on the network For instructions refer to the installation guide for the h
60. lamp has been in service for more than 1000 hours If this occurs replace the lamp see Section 5 7 Tungsten lamp needs replacement Install a new tungsten lamp see Section 5 8 Lamp incorrectly installed Make sure that both lamps are fully seated in the optical bench See Section 5 7 or Section 5 8 for installation instructions for the deuterium lamp or tungsten lamp respectively Inappropriate reference wavelength Select a reference wavelength in a quiet area of the spectrum 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 Section 3 4 4 4 Doc 031644 02 9 03 de Troubleshooting e Bandwidth is too narrow Select a wider sample bandwidth and reference bandwidth if appropriate for the application For guidelines when selecting the sample and reference bandwidths see Section 3 4 Flow cell cover lamp cover or front panel is missing Optical components are sensitive to temperature and light Do not operate the PDA 100 unless the flow cell cover lamp cover and front panel are in place Crimped or plugged tubing Over time tubing may become pinched off and plugged Periodically check all tubing and replace as needed see Section 5 1 Flow cell installed incorrectly Be sure the cell is inserted straight into the optical bench and is fully seated see Section B 4 2
61. lengths 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 run 1 2 Doc 031644 02 9 03 1 Introduction e Determination of the correct wavelengths one run After all peaks have been detected the maximum absorbance wavelength for each peak can be determined A PDA detector can collect spectra of each peak and 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 e 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 A pure peak has matching spectra throughout the peak at all wavelengths Positive peak identification In liquid chromatography peak identification is usually based on relative retention times When a PDA detector 1s 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 impuri
62. m 800 nm to 350 T T T T T T T T T 338 350 363 375 388 400 413 425 438 nm 450 BI 84 E g E EE EE 272 nm Sample Wavelength 325 nm Reference Wavelength Figure 3 6 Caffeine Spectrum e 031644 02 9 03 3 23 PDA 100 Photodiode Array Detector 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 nm will reduce the required data storage by the reciprocal For example a bunch width of 5 nm requires one fifth the amount of storage as a bunch width of 1 nm This parameter reduces the spectral resolution so do not select a bunch width when the spectrum of the compound has a fine structure Step IMPORTANT The appropriate PDA 100 step setting is automatically selected by the software A step is the time interval between two successively stored data points The smaller the step the more data points that are recorded and in general the more precise the analytical results However because collecting more data points requires more storage capacity the step setting sometimes represents a compromise between the amount of information collected and the file size The user does not need to select a step setting PeakNet 6 or Chromeleon automatically selects the step value that is the inverse of the data collection rate For example if you set the data collection rate to 5 0
63. m 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 0 25 mm 0 010 in ID tubing to the required length The backpressure line should be meter long for a flow rate of 1 0 mL min 2 meters for 0 5 mL min and so on c Install a ferrule fitting and 10 32 bolt on each end of the tubing d Install the backpressure line after the cell outlet Use a union P N 042627 to connect the backpressure line to the waste line Cell Inlet Tubing Cell Outlet Tubing Flow Cell Heat Exchangers Spring Clip 5 Figure B 2 Flow Cell Connections The cell connections exit the detector through slots in the front panel 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 front panel into place Connect the cell outlet tubing to the separator column outlet IMPORTANT Operating at backpressures greater than 2 MPa 300 psi or 3 MPa 500 psi will damage the PEEK or stainless steel cell heat exchanger respectively B 4 Doc 031644 02 9 03 B Installation B 3 3 B 3 4 Waste Line Connect the waste line P N 054779 to the PDA 100 rear panel see Figure B 1 Place the free end of the line in a waste container below the level of the lab bench on which the PDA 100 is installed The drain tube must remain below the drain port If th
64. matograms with co eluting peaks or low signal to noise ratios 40 data points per peak is recommended If all peaks are relatively wide select a slower data collection rate 1 0 Hz for example If any peaks of interest are less than a few seconds select a faster data collection rate 5 0 Hz for example If the data collection rate is too slow the start and end points of peaks are not accurately determined However if the collection rate is too fast data files may occupy excessive disk space and post run analyses may require more processing time A slow data collection rate with a fast rise time may result in a longer system response than indicated by the rise time For example a data collection rate of 0 5 Hz and arise time of 0 5 second results in a system response longer than 2 0 seconds The table below lists the recommended pairings for the rise time and data collection rate Rise Time Data Collection Rate seconds Hz 0 1 10 0 0 2 10 0 0 5 5 0 1 0 2 5 2 0 2 0 5 0 0 5 Doc 031644 02 9 03 3 17 PDA 100 Photodiode Array Detector Sample Wavelength The PDA 100 measures absorbance over all wavelengths from 190 nm to 800 nm The deuterium lamp optimizes the UV range 190 nm to 380 nm The tungsten lamp optimizes the visible range 380 nm to 800 nm Set the sample wavelength at the wavelength with the absorbance maxima When the analyte wavelength maximas are known the detector can run five separate
65. me Diagnostics The PDA 100 Moduleware periodically checks the status of certain system parameters Minor problems that do not justify stopping operation are reported to the host computer and recorded in the Audit Trail The Audit Trail includes the date time and error code 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 and the file for that date Software Diagnostics and Calibration PeakNet 6 and Chromeleon contain comprehensive diagnostics for the PDA 100 This section briefly describes some of these diagnostics for a full description refer to the software Help or user s manual Lamp age Indicates the total number of hours that each lamp has been turned on in its lifetime To reset the lamp age after installing a new lamp a Press F8 to display the Commands dialog box b Select UV to display UV related commands c Select UVLampAge or VisLampAge Reset the number to zero e Click the Execute button NOTE When the detector power is initially turned on the lamp age already indicates some elapsed time this is the time required for factory calibration and test procedures 4 14 Doc 031644 02 9 03 de Troubleshooting Wavelength calibration Reassigns new wavelengths to each pixel based on the emission spectrum f
66. mperature Operating Humidity Electrical Main Power Fuses 4 C to 40 C 40 F to 104 F 5 to 95 relative humidity noncondensing 85 Vac to 264 Vac 47 63 Hz The input power is 162 W maximum the output power is 130 W maximum The maximum input current is 4 amps The auto sensing power supply requires no voltage or frequency adjustment Two 4 0 amp fast blow IEC 127 fuses P N 954763 Doc 031644 02 9 03 PDA 100 Photodiode Array Detector A 4 Detector Optical System Light Sources Photodiode Array Wavelength Range Pixel Resolution Wavelength Accuracy Noise Drift Linearity Analog Outputs Voltage Out Analog Output Range Control and Data Evaluation Single beam reverse optics design with concave holographic grating Deuterium lamp 30 W for ultraviolet spectrum analysis Tungsten lamp 15 W for visible spectrum analysis 1024 elements 190 nm to 800 nm 0 7 nm 1nm 10 with 2 second rise time 254 nm 4 nm bandwidth and flowing deionized water 15 with 2 second rise time 520 nm 10 nm bandwidth and flowing deionized water lt 500 pAU hour after warm up gt 2 AU Four built in analog outputs 1 V output 0 0005 0 001 0 01 0 1 0 5 1 0 2 0 or 3 0 AU full scale Provided by PeakNet 6 or Chromeleon software communication with the detector is via the DX LAN interface Doc 031644 02 9 03 A Specifications A 5
67. n 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 separated into its component wavelengths and diffracted to the photodiode array Each diode measures a narrow portion of the spectrum Visible Focus Lens Tungsten Lamp x m oe SA Deuterium Lamp Flow Cell Filter SSR AS Photodiode A S AM Lens ATV Spectrograph Lens Grating de KS Figure 2 3 PDA 100 Optical System 2 4 Doc 031644 02 9 03 2 Description Optical System Component Tungsten Lamp Visible Focus Lens Deuterium Lamp Source Lens Flow Cell Spectrograph Lens Filter Paddle Slit Grating Photodiode Array Function The light source for visible and near infrared wavelengths 380 nm 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 nm to 380 nm also used to check the wavelength calibration Receives the light from the tungsten and deuterium lamps and focuses it so that the beam passes through the flow cell The measurement sit
68. ngth Cell Volume Heat Exchanger Volume PEEK 10 mm 13 uL 20 uL P N 056346 Stainless Steel 10mm 13 uL 9 uL P N 056126 IMPORTANT Do not touch the cell windows If you touch a window clean it with denatured alcohol and a clean lens tissue Do not use the PEEK flow cell with normal phase or chlorinated IMPORTANT solvents these solvents will damage the cell Do not use the stainless steel flow cell with high pH salts the salts IMPORTANT SSES can cause corrosion contamination and metal leaching 2 6 Doc 031644 02 9 03 2 Description 2 4 Electronics Do not attempt to access the PDA 100 electronics The components on the cards 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 MISEEN 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
69. omputer Flashing An alarm was activated for example the leak sensor in the drip tray may have been triggered Off Data is not being acquired by the host computer 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 5 Off The deuterium lamp is off Doc 031644 02 9 03 2 1 PDA 100 Photodiode Array Detector LED LED Status Function 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 5 Off The tungsten lamp is off Power Lighted The detector power is on Press the Power switch to turn the detector on and off Flashing The detector failed one of the electrical checks or optical checks performed during the power up sequence see Section 4 15 1 Off The detector power is off Press the Power switch to turn the detector on and off 2 2 Doc 031644 02 9 03 2 Description 2 2 Inside Front Panel NOTE For an illustration of the inside front panel with the flow cell cover and lamp cover removed see Figure 5 1 Grasp the PDA 100 front panel by the sides and pull straight off to access the inside front panel see Figure 2 2 Power e Switch 6 DEL EL
70. on is required in order to perform the following 3D data presentation and spectral analysis spectral library search for positive peak identification and peak purity analysis with selectable criteria 3 3 1 Panel Control In this mode the user selects PDA 100 operating parameters and commands from a control panel in the software Commands are executed as soon as they are entered and 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 PeakNet 6 or Chromeleon online Help or user s manual Summary of control panel operation 1 Start PeakNet 6 or Chromeleon 2 Open the Browser 3 Select one of the PDA 100 default control panels e DIONEX PUMP PDA AUTOSAMPLER PAN the 2D control panel monitors chromatograms of up to five signals see Figure 3 1 e DIONEX PUMP PDA3D AUTOSAMPLER PAN the 3D control panel monitors chromatograms contour plots and spectra on line see Figure 3 2 The 3D control panel is available only when PeakNet 6 or Chromeleon includes the 3D option Doc 031644 02 9 03 3 5 PDA 100 Photodiode Array Detector Connect the control panel to the timebase Select the operating parameters Turn on the pump Set the flow rate and mobile phase composition B Click the Acquisition On Off toolbar button to begin manual data acquisition 8 Click the Acquisition
71. onnections 16 Replace the flow cell cover and reconnect the inlet and outlet tubing IMPORTANT Do not pinch the tubing under the flow cell cover 17 Replace the detector front panel 18 Turn on the detector power 19 Start the PeakNet 6 or Chromeleon server Doc 031644 02 9 03 5 7 PDA 100 Photodiode Array Detector 20 Reset the lamp lifetime as follows a b d e NOTE Press F8 to display the Commands dialog box Select UV to display UV related commands Select UVLampAge Reset the lamp age to zero Click the Execute button It is normal for the baseline to drift for several hours after a new deuterium lamp is installed 2 Runthe wavelength calibration and verification for the new lamp from the Wellness panel see Section 4 15 2 Doc 031644 02 9 03 5 e Service 5 8 Replacing the Tungsten Lamp 1 Stop the PeakNet 6 or 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
72. ow cell cover and front panel are in place optical components are sensitive to temperature and light 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 Lamp not stabilized The lamps usually require 20 to 30 minutes to stabilize For sensitive applications work or for detector validation allow at least 2 hours for the lamps to stabilize After installing a new lamp allow from 8 to 24 hours for the lamp to stabilize After changing mobile phases allow 20 to 30 column volumes for the system to stabilize Leaking flow cell Tighten fittings if the cell continues to leak replace it Also check that the backpressure on the cell does not exceed the specification see Section A 5 Inappropriate reference mode selected Dionex recommends selecting a reference wavelength active reference mode for gradient analyses and turning off the reference wavelength for Doc 031644 02 9 03 de Troubleshooting isocratic analyses in a laboratory with a stable ambient temperature For more information see Section 3 4 e Absorbance in the reference wavelength Sample absorbance in the selected reference wavelength may cause excessive baseline drift Select a reference bandwidth in an area of the spectrum where little absorption occurs see Section 3 4 Dionex recommends selecting a referenc
73. power source Check the fuses and replace them if necessary see Section 5 9 Power up sequence failed If the Power LED is flashing turn off the detector power briefly Turn on the power again and check that the Power LED is lighted but is not flashing Lamp not turned on If a lamp is turned off the corresponding front panel LED Deuterium or Tungsten is off also Turn on the lamp from the software or the TTL input Lamp LED flashing The lamp did not power on properly Press F8 in the software to display the Commands dialog box select UV to display UV related commands and check that UVLampPowerOnSetting and VisLampPowerOnSetting are Off If the LED continues flashing replace the lamp s See Section 5 7 or Section 5 8 for replacement instructions for the deuterium lamp or tungsten lamp respectively PDA 100 not detected on the DX LAN When the host computer is powered up the software scans the DX LAN for all installed instruments If the PDA 100 power is off the detector cannot be identified Before turning on the computer make sure the detector power is already turned on DX LAN interface incorrectly installed Check the following for installation instructions see Section B 3 6 e 10BASE T DX LAN cable P N 960281 must be connected between the DX LAN connector on the PDA 100 rear panel and the Ethernet hub P N 056909 4 2 Doc 031644 02 9 03 de Troubleshooting e A 10BASE T DX LAN cable P
74. r the PDA 100 and is easily accessible gt CAUTION 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 sich die Steckdose nahe am Ger t befindet und leicht zuganglich ist gt VORSICHT The PDA 100 power supply is auto sensing so it is not necessary to manually select the line voltage or frequency To control power to the detector connect a modular power cord IEC 320 C13 from the PDA 100 main power receptacle see Figure B 1 to a grounded single phase power source Use the PDA 100 power switch see Figure 2 1 to turn the detector on and off B 2 Doc 031644 02 9 03 B Installation PDA
75. ression 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 Doc 031644 02 9 03 3 1 PDA 100 Photodiode Array Detector 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 do not let buffers remain in the cell for extended periods 3 1 2 Solvent Delivery System The pumping system should deliver continuous flow while maintaining a consistent mobile phase composition if gradient elution is used Fluctuations in system backpressure may cause 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 extremes of pH or with high salt concentration 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 moder
76. rom the deuterium lamp Both the initial calibration and previous calibration are stored in the calibration log and can be retrieved at any time To calibrate the wavelength a b Press F8 to display the Commands dialog box Select UV to display UV related commands Select UV_Calibration and then WavelengthCal Click the Execute button When the calibration procedure is complete select the WavelengthCalResult command or click the Wavelength button on the PDA 100 Wellness control panel Doc 031644 02 9 03 PDA 100 Photodiode Array Detector 4 16 Doc 031644 02 9 03 5 Service This chapter describes routine service procedures that the user may perform procedures not described here must be performed by trained Dionex Service personnel 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 cannot be serviced by the user all repairs of these components must be performed by trained Dionex Service personnel The Data Processing card contains lithium battery If the card is amp KY replaced dispose of the used battery according to local regulations ens 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 thereb
77. ry search for positive peak identification e Optimal integration path determination for method optimization 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 whereas photodiode array PDA detectors scan a range of wavelengths every few milliseconds and continually generate 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 run 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 run 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 wave
78. s Document No 031152 Doc 031644 02 9 03 3 29 PDA 100 Photodiode Array Detector Replace the deuterium and tungsten lamps when required see below The average lamp lifetime is 1000 hours However lamps often last longer than this with only minimal deterioration in performance Monitor baseline noise If the noise increases above an acceptable level especially after a lamp s has been in service for more than 1000 hours replace the lamp See Section 5 7 or Section 5 8 for replacement instructions for the deuterium or tungsten lamp respectively Approximately every 6 months check the intensity of the deuterium lamp as follows Press F8 in PeakNet 6 or Chromeleon to display the Commands dialog box select UV to display UV related commands and select LampIntensity The reading should be above 10 million counts if it is not select the UV_Calibration Intensity command to calibrate the lamp After calibration 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 Approximately every 6 months run the wavelength calibration and verification procedures for the deuterium and tungsten lamps from the Wellness panel see Section 4 15 2 Doc 031644 02 9 03 4 Troubleshooting This chapter is a guide to troubleshooting routine problems that may occur while operating the PDA 100 Photodiode Array Detector Turn to the section that best d
79. s approximately 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 iil T L db nn li d li ui d TT N WII W IW JEM Wn Ko di ii IM ii Rise Time 2 0 sec Baseline Noise 10 AU d A V A 1 0 0000 W N d Vii IM hi A In M n G l KE MI IN vlt lag Li V Nu M dn Vi 0 0100 gd Y Figure 3 3 Effect of Rise Time on Baseline Noise 3 16 Doc 031644 02 9 03 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 host computer stores data from the PDA 100 The detector electronics always collect data at 10 0 Hz The data collection rate can be set to 0 25 0 5 1 0 2 0 2 5 default 5 0 or 10 0 Hz The maximum number of data points 1s stored at 10 0 Hz Slower data collection rates store the average of the 10 0 Hz points for example a 2 5 Hz rate stores the average of four 10 0 Hz points In general each peak should be defined by at least 20 data points For chro
80. s are guidelines only After changing the negative absorbance setting run autozero and then check the intensity of the deuterium lamp Press F8 to display the Commands dialog box select UV and select LampIntensity The reading should be above 10 million counts if it is not select the UV Calibration Intensity command to calibrate the lamp After calibration 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 Negative Approximate Negative Approximate Negative Approximate Negative Absorbance Absorbance at210nm Absorbance at240nm Absorbance at 254 nm Level 0 1 2200 mAU 50 mAU 300 mAU 2300 mAU 100 mAU 350 mAU 2600 mAU 200 mAU 450 mAU 2600 mAU 300 mAU 550 mAU 2700 mAU 400 mAU 630 mAU 2700 mAU 500 mAU 660 mAU 2700 mAU 600 mAU 760 mAU These signals are saturated and will not report a further negative value Doc 031644 02 9 03 3 27 PDA 100 Photodiode Array Detector 3 5 Stand Alone Analog Operation This section describes limited stand alone detector operation when the PDA 100 is not interfaced to a host computer running either PeakNet 6 or Chromeleon software In stand alone operation TTL inputs can be used to trigger autozero or turn the deuterium and tungsten lamps on and off All other detector parameters remain at their factory default settings and cannot be changed Factory Defaults The PDA 100
81. sed lock on each side of the fuse holder now using a small screwdriver or your fingernails push one of the locks toward the center to release it The fuse holder pops out slightly when the lock is released Repeat for the other lock Fuse Holder Fuses 2 E d Key gt Fuse Holder Side View Locking Spring Insert screwdriver and twist to release each side Main Power Receptacle Figure 5 4 Main Power Fuse Holder Doc 031644 02 9 03 5 11 PDA 100 Photodiode Array Detector 4 When both locks are released pull the fuse holder straight out of the compartment and replace the two fuses in the holder with new 4 0 amp fast blow IEC 127 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 panel 6 Reconnect the power cord and turn on the power 5 12 Doc 031644 02 9 03 A 1 Physical Dimensions Weight Decibel Level A Specifications 17 5 cm H x 38 6 cm W x 49 0 cm D 6 9 x 15 2 x 19 3 in 6 cm 2 4 in clearance required behind the detector 16 kg 35 Ibs lt 50 db at A WEIGHTING setting during routine operation 56 db at A WEIGHTING setting at power up A 2 Environmental Operating Te
82. tionLevel setting to shift the detection level This is especially helpful when running a gradient application in which the absorbance decreases more than several hundred mAU For example in Figure 3 7 the NegativeAbsorptionLevel setting is 100 initially and the baseline is flat when the gradient 15 5096 The baseline is not flat when the gradient is gt 5 and the NegativeAbsorptionLevel is set to 600 Chromeleon 685011 _ 010401 Miles Apr O3 NEGATIVE ABSORBANCE_10APRO3 29 Caffeine Gradient UY VIS 3 68Kso11_backW10401 la f e Edt View Workspace Qualification Widow Help dmi iE 88 87 iN PAE UV vis 3 NegativeAbsorptionLevel 100 V a g 1 50 NV N 25 NegativeAbsorptionLevel 600 Figure 3 7 Gradient Baseline with NegativeAbsorptionLevel Settings of 100 and 600 3 26 Doc 031644 02 9 03 3 Operation and Maintenance In PeakNet 6 or Chromeleon press F8 to display the Commands dialog box Select UV select the NegativeAbsorptionLevel command and select a higher setting You may continue increasing the setting if the range is required Baseline noise may increase as the NegativeAbsorptionLevel setting increases At the default setting the detector will become saturated when the light transmission is 20 above the autozero level The extent of negative absorbance is wavelength dependent as indicated in the table below these value
83. troke the piston seal or check valves may need cleaning Refer to the pump user s manual for instructions 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 Doc 031644 02 9 03 4 3 PDA 100 Photodiode Array Detector Plot scale exaggerates baseline noise If autoscale is selected even a plot with low noise may fill the screen Check the Y axis values Air bubbles in flow cell Remove the trapped air see Section 5 3 To prevent air from becoming trapped in the cell 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 2 This increases the backpressure thereby shrinking bubbles and allowing them to pass more easily through the cell Contaminants in flow cell Clean the cell see Section 5 2 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 Deuterium lamp is dimming The light output of the deuterium lamp decreases over time The lower light output may increase noise above an acceptable level especially after the
84. ttention to certain information They alert the user to an unexpected result of an action suggest how to optimize instrument performance etc Doc 031644 02 9 03 PDA 100 Photodiode Array Detector 1 4 Safety 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 1993 safety CAN CSA C22 2 No 1010 1 92 safety UL 3101 1 10 93 safety EN 50082 1 1992 susceptibility and EN 55011 1991 emissions These symbols appear on the PDA 100 or on PDA 100 labels ES Alternating current D Protective conductor terminal Power supply is on C Power supply is off 1 8 Doc 031644 02 9 03 21 Front Panel 2 Description Figure 2 1 illustrates the front panel of the PDA 100 Photodiode Array Detector The Power switch provides on off control of the detector power LED indicators identify the status of four functions the detector power the deuterium and tungsten lamps and the run A solid lighted LED indicates that the corresponding function is in progress A flashing LED indicates that an error occurred for an explanation check the Audit Trail in PeakNet 6 or Chromeleon DIONEX Run Deuterium Tungsten Power PDA 100 Photodiode Array Detector Figure 2 1 PDA 100 Front Panel LED LED Status Function Run Lighted Data is being acquired by the host c
85. ty obtained from two consecutive chromatographic runs Based on 2D data or if the run had been performed with a conventional variable wavelength detector these peaks would have been misidentified as the same component A PDA 100 under the control of Dionex software with the 3D option correctly identified and differentiated the components The spectra of pyrene and the impurity see Figure 1 2 clearly indicate that the two peaks are different components Doc 031644 02 9 03 1 3 PDA 100 Photodiode Array Detector 1 Calibration 5 Solvent Injection 222 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 Doc 031644 02 9 03 1 Introduction 1 3 About 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 Provides a brief overview of the PDA 100 and the theory of photodiode array detection Summarizes the organization of the user s manual Explains the meaning of safety messages and icons
86. ub Doc 031644 02 9 03 Part Number 939016T 056123T 954763 923686 043598 056346 060037 043276 043275 060498 056126 060038 055902 010262 010261 060498 C Reordering Information Item Deuterium Lamp Tungsten Lamp Fuse 4 amps Fast Blow IEC 127 12 Pin Relay TTL Connector Twisted Wire Assembly PDA 100 with PEEK Flow Cell PEEK Flow Cell with heat exchangers PEEK Flow Cell Outlet Tubing Assembly Ferrule Nut Flow Cell Windows Replacement Kit PDA 100 with Stainless Steel Flow Cell Stainless Steel Flow Cell with heat exchangers Stainless Steel Flow Cell Outlet Tubing Assembly Union Fitting Ferrule Nut Flow Cell Windows Replacement Kit Quantity 1 1 1 2 m 8 ft Fe Se Se Lm ke Se Se Se Se Se Ee Doc 031644 02 9 03 C 1 PDA 100 Photodiode Array Detector C 2 Doc 031644 02 9 03 Numerics 2D data 1 1 3D data 1 2 3 5 3 18 Bunch width selection 3 24 Reducing data file size 3 25 Software support 1 2 3 5 Step time selection 3 25 A Absorbance calculation 3 23 Absorbance range 2 12 Active reference mode 3 20 See also Reference wavelength Selecting 3 20 Turning off 3 20 Air bubbles in cell Preventing 4 4 B 4 Removing 5 2 Air conditioning 3 20 Ambient temperature fluctuations 3 20 Analog output connectors 1 1 2 9 2 12 Default settings 3 28 Analog output range 2 12 Analytes unknown 3 18 Audit Trail 2 1 4 1 Autoscale 4 4 Autozero
87. ule fittings 4 3 Installation instructions 5 1 Part number B 4 Index 2 Doc 031644 02 9 03 Index Filter paddle 2 4 2 5 Malfunction 4 5 Positions 2 5 Flow cell See Cells Front panel Illustration 2 1 LEDs described 2 1 2 2 Fuses 2 11 A 1 Replacing 5 11 G Gradient analyses Reference wavelength selection 3 20 4 6 4 7 Gradient applications 3 26 Grating optical 2 4 2 5 H Heat exchangers 2 6 Operating pressure A 3 Pressure specification B 4 Volume 2 6 A 3 Holmium oxide filter 1 1 2 5 Filter paddle positions 2 5 Wavelength verification 2 5 Hub 10BASE T 4 2 4 10 B 8 Cascading hubs B 8 Part number 4 2 4 10 B 8 Humidity operating A 1 I Important icon 1 6 B 8 Inside front panel 2 3 Access to panel 2 3 Illustration 2 3 Installation Instructions B 3 B 5 B 7 Site requirements A 1 B 1 Integrator 4 11 B 5 Isocratic analyses Reference wavelength selection 3 20 4 7 L Lamp power supply 2 8 Lamps 1 1 Calibration 4 8 Deuterium LED flashing 2 1 Failure 2 1 2 2 Installation procedures 5 6 5 9 Maintenance 3 30 See also Deuterium lamp See also Tungsten lamp Tungsten LED flashing 2 2 Leak alarm 2 3 Leak sensor 2 3 Leak tray 2 3 Maintenance 2 12 3 29 Leaks 2 3 Prevention 2 12 Symptoms 3 29 LEDs on front panel 2 1 2 2 Lenses 2 5 Liquid lines Maintenance 3 29 Lithium battery disposal 5 1 Location 2 3
88. w an Wechselstrom angeschlossen WARNUNG werden Stellen Sie sicher sich die Steckdose nahe am Ger t befindet und Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung As leicht zug nglich ist VORSICHT Fuses The PDA 100 uses two 4 0 amp fast blow fuses IEC 127 type 1 P N 954763 See Section 5 4 for fuse replacement instructions For continued protection against risk of fire or shock replacement fuses must be the type and rating specified here WARNING Pour maintenir la protection contre les risques d incendie ou d lectrocution remplacez toujours les fusibles par des fusibles du m me type et du m me calibre gt AVERTISSEMENT Zum Schutz vor Feuer und Stromschlagen m ssen beim Sicherungswechsel immer Sicherungen des gleichen Typs und mit gleicher Leistung verwendet werden WARNUNG Doc 031644 02 9 03 2 11 PDA 100 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 selected from the software includes 0 0005 0 001 0 01 0 1 0 5 1 0 2 0 and 3 0 AU full scale For details about programming the analog outputs see Section 3 3 2 The analog outputs continue to output data even after the host computer is turned off or is disconnected from the PDA 100 When the detector power is turned on again the analog output settings are either the factory defaults s
89. wavelengths without being required to collect spectra Collecting individual wavelengths instead of the spectra offers two advantages it saves disk space when 3D data is not required and it eliminates the need to perform extractions for runs that do not require spectral data If little is known about the analytes in the sample collect spectra over the full wavelength range using both lamps Although this requires more disk space it provides complete information about the analytes and the spectra can be used to determine peak identity purity and wavelength maxima Doc 031644 02 9 03 3 Operation and Maintenance Sample Bandwidth The sample bandwidth is the wavelength range at which the chromatogram is measured As the bandwidth increases baseline noise decreases Increasing the bandwidth increases the number of wavelength signals overlaid at each point in time Increasing the bandwidth may also decrease the signal especially of those peaks with narrow peak maximas Select a sample bandwidth that provides the resolution required to achieve the desired sensitivity Selecting a wider bandwidth reduces baseline noise but may also reduce peak height For narrow spectral peaks select narrow bandwidths Example Chromatogram Selecting the Bandwidth Figure 3 4 illustrates how selecting a wide bandwidth for both the sample and reference reduces noise by averaging over a wavelength range The operating conditions are Sample wav
90. width setting of 1 nm and then recheck the resolution Sample bandwidth too wide Select a sample bandwidth that includes only the absorbing wavelength 4 10 Doc 031644 02 9 03 de Troubleshooting Incorrect reference wavelength Select a reference wavelength where minimum absorbance occurs Make sure the reference wavelength is included in the wavelength range Wavelength range too narrow Make sure the spectrum wavelength range includes both the reference wavelength and reference bandwidth Make sure the peak absorbance wavelength is not included in the reference bandwidth Reference bandwidth too wide Select a narrower reference bandwidth The reference bandwidth should not overlap the sample 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 and data collection rate are appropriate to capture the narrowest peak See Section 3 4 for more information Prepare fresh post column reagent Verify that the reagent flow rate is correct Reference bandwidth too wide Select a narrower reference bandwidth The reference bandwidth should not overlap the sample bandwidth Doc 031644 02 9 03 4 11 PDA 100 Photodiode Array
91. 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 PeakNet 6 or Chromeleon server 19 Reset the lamp lifetime as follows a Press F8 to display the Commands dialog box b Select UV to display UV related commands c Select VisLampAge d Reset the lamp age to zero e Click the Execute button NOTE Before resuming routine operation allow 20 to 30 minutes for the lamp to stabilize 5 10 Doc 031644 02 9 03 5 e Service 5 9 Replacing the Main Power Fuses HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the PDA 100 DANGER HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau du PDA 100 DANGER HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite des PDA 100 ACHTUNG 1 Turn off the PDA 100 power switch 2 Disconnect the power cord from the PDA 100 rear panel 3 The fuse holder is part of the main power receptacle see Figure 5 4 Note the reces
92. y voiding the product warranty Refer to the warranty statement in the Dionex Terms and Conditions for more information 5 1 Liquid Leaks The PDA 100 is plumbed with the components listed below For tightening requirements refer to Installation of Dionex Ferrule Fittings PDA 100 with PDA 100 with Component PEEK Flow Cell Stainless Steel Flow Cell Tubing 0 25 mm 0 010 in ID P N 042690 P N 019245 Union Fittings P N 055903 P N 055902 Ferrules P N 043276 P N 010262 Nuts P N 043275 P N 010261 Doc 031644 02 9 03 5 1 PDA 100 Photodiode Array Detector 5 2 5 3 Cleaning the Flow Cell Film deposits on the flow cell windows may cause excessive baseline noise or high absorbance offset 1 Pump methanol through the cell for 20 to 30 minutes at 1 0 mL min 2 Pump deionized water through the cell for 20 to 30 minutes at 1 0 mL min If the procedure above does not clean the cell follow these steps 1 Disconnect the liquid lines from the cell in and out connections 2 Connect luer adapter to the cell in connection 3 Using a syringe flush the cell with a succession of deionized water acetone M HNO3 4 Flush the cell with deionized water for 20 to 30 minutes at 1 0 mL min 5 Reconnect the cell liquid lines 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

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