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UltiMate 3000 Series Photodiode Array Detector

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1. Operating Instructions Page 37 UltiMate 3000 Series Photodiode Array Detector Program Wizard Select Timebase Options PD4 3000 i MELAB 1 5 35 Network Neighborhood My Computer Fig 20 Program Wizard Selecting the Timebase 3 Select the Timebase where the program will run 4 Click Next to continue If the selected timebase includes other devices pump detector etc Program Wizard screens for these devices precede the PDA 3000 screens Click the Next button on each screen for another device until the Acquisition Options screen appears Program Wizard Acquisition Options 30 000 Fig 21 Program Wizard Acquisition Options 5 To determine for how long data will be collected specify when the Acquisition Time starts and ends Page 38 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 6 Select the channels and or devices for which data will be collected To enable or disable all entries listed here click Select All or Deselect All respectively T 8 Click Next to continue The following screen is displayed Program Wizard UY Options xi Data Collection Rate M 0 25 20 00 Hz Rise Time 200 gt 0 05 5 00 s Start settings and data acquisition times Channel name AeqOn min Acqoffimin Wavel nm Bandw nm m MUV VIS 1 0 000 30 000 210 10 am MUV VIS 2 0 000 30 000 254 10 0 Ea m UY VIS 3 0 000 30
2. Page 88 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 6 2 5 Replacing the Flow Cell Windows and Seals The description below refers to analytical and semimicro flow cells only The windows in the semipreparative flow cell cannot be replaced by the user If cleaning the cell does not eliminate the problems described above replace the entire cell Description Part No Flow cell windows replacement kit including 6080 1200 2 flow cell windows 2 O ring seals windows replacement tool NOTE Contaminated flow cell windows can significantly increase baseline noise and cause wavelength calibration to fail If cleaning the cell section 6 2 2 page 86 does not eliminate these problems replace both silica windows 1 Remove the flow cell from the optical bench section 6 2 4 page 87 and place the cell on a clean work surface 2 Put ona pair of latex gloves Important Even minute particles of dust dirt etc on the flow cell parts can contaminate the cell and result in excessive baseline noise and drift 3 Using the windows replacement tool from the replacement kit remove one of the flow cell retaining nuts from the flow cell Fig 31 It does not matter which retaining nut is removed first RQ lt lt Cell Outlet Tubing v Cell Inlet Tubing N O Ring Groove r f O Ring gt Window SX Flow Cell Retaining Nut Fig 31 Rep
3. For example you may want to increase the step time for the 3D field or any of the five absorbance channels For the 3D field the step determines the sampling rate at which the detector stores spectra Ideally the step is no smaller than the interval suggested for the rise time see the table in the Data Collection Rate section on page 46 The advantage of a larger step size is that it reduces the amount of data stored for example selecting a step twice as large as that listed in the table reduces the data file size for the 3D field by 50 If you select a larger step size when the average parameter is on see the Average section below the system response is a combination of the selected rise time and the average of the data points between steps If you select a larger step size when the average parameter is off the selected rise time is valid but some data points will be skipped 4 3 10 Average The Average parameter operates in conjunction with the Step parameter see the Step section on page 52 When Average is On Chromeleon averages the data points between Step intervals reports that value and noise is reduced This setting is recommended for most applications When Average is Off Chromeleon reports the data points at the step interval The data points between steps are skipped and noise is not reduced If the step size is more than double the rise time the system response is dominated by the step size The system r
4. Fuse holder Fig 37 Main Power Receptacle Replace the two fuses in the holder with new 4 0 amp fast blow IEC 127 fuses Dionex recommends always replacing both fuses Do not operate the detector with only one fuse 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 lock is engaged When correctly installed the fuse holder is flush against the rear panel Reconnect the power cord to its source and turn on the detector Operating Instructions Page 97 UltiMate 3000 Series Photodiode Array Detector Page 98 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 7 Specifications Noise with Analytical or Semipreparative Cell Installed Noise with Semi Micro Cell Installed Drift Wavelength range Wavelength accuracy Resolution Linearity Analytical flow cell Semi micro flow cell Semipreparative flow cell Maximum cell pressure Optical System PEEK cell 13 uL volume 10 mm 0 394 in path length PEEK cell 3 1 uL volume 9 mm 0 35 in path length Photodiode array Pixel resolution lt 10 pAU at 254 nm 2 second rise time 4 nm bandwidth and flowing water at 1 0 mL min lt 15 AU at 520 nm 2 second rise time 10 nm bandwidth and flowing water at 1 0 mL min lt 15 AU at 254 nm 2 second rise time 4
5. page 16 and is correctly connected to the inside front panel Fig 31 page 89 Check that solvent flow is directed to the cell inlet and out the cell outlet Semi micro cell flow rate selected when analytical cell is installed For operation at less than 1 0 mL min install a semi micro flow cell 5 14 Faulty USB Communication PDA 3000 not recognized by Windows operating system Dionex strongly recommends installing Chromeleon before connecting the PDA 3000 to the computer When the software is installed first USB driver information is loaded automatically If you connect the PDA 3000 to the computer before installing Chromeleon a Windows message box requesting a USB configuration file cmwdmusb inf will appear when you turn on the computer Follow these steps to resolve the problem 1 Click Cancel in the Windows message box 2 Turn off the power to the PDA 3000 and unplug the USB cable from the computer 3 Install Chromeleon 4 Reconnect the USB cable to the computer and turn on the power to the PDA 3000 Windows will now automatically recognize the detector Operating Instructions Page 81 UltiMate 3000 Series Photodiode Array Detector Page 82 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 6 Routine Maintenance This chapter describes routine service procedures that users may perform All procedures not described here must be performed by Dionex Service personnel NOT
6. 2 Open the detector front panel 3 Remove the flow cell from the optical bench page 87 NOTE It is not required to disconnect the flow cell from the fluidic flow 1 e step 1 from the description of how to remove the flow cell can be omitted 4 Move the flow cell tubing out of the way Remove the four screws holding the lamp cover Fig 34 page 92 in place and then remove the cover and set it aside 5 Remove the two crosshead screws that hold the metal connector cover on the right Fig 34 page 92 and then remove the cover and set it aside 6 Squeeze the clip on the visible lamp connector and disconnect it from the 4 pin bulkhead connector on the side wall Fig 35 page 93 7 Use a screwdriver to loosen the tungsten lamp screws and then pull the mounting assembly away from the optical bench NOTE The screws are captive in the lamp base and do not need to be removed 8 Inspect the new tungsten lamp for fingerprints and dust If necessary clean the lamp with isopropyl alcohol 9 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 Operating Instructions Page 95 UltiMate 3000 Series Photodiode Array Detector 10 11 12 13 14 15 16 Squeeze the clip on the Vis lamp connector and inser
7. 30 page 88 Fig 15 Threading the inlet tubing through the tubing guide 6 Thread the flow cell outlet tubing through the slot on the side of the flow cell cover Replace the cover and tighten the two screws on the cover fingertight Do not pinch the tubing under the flow cell cover 7 Optional Connect a backpressure line to the cell outlet connection The backpressure line will provide enough restriction to generate the small amount of backpressure 0 14 to 0 34 MPa 20 to 50 psi required to help prevent bubbles from forming in the cell If you decide to connect a backpressure line you do not have to connect an outlet capillary as described in step 8 a The flow cell is shipped with a 2 meter 0 25 mm 0 010 in ID capillary for the backpressure line b Cut the tubing to the required length The backpressure line should be 1 meter long for a flow rate of 1 0 mL min 2 meters for a flow rate of 0 5 mL min and so on c Connect the backpressure line to the cell out connection The backpressure on the cell must not exceed 21 bar 300 psi for a PEEK analytical or semi micro cell 35 bar 500 psi for a stainless steel analytical or semi micro cell or 100 bar 1450 psi for a semipreparative cell Page 32 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 8 The flow cell is shipped together with a 0 5 m capillary and hose to be connected to the cell outlet connection Connect this liquid line
8. If you have already selected these parameters on the device page for a particular module the list box on the Relay and State Devices Options page already contains this information If you change any settings here Chromeleon will automatically copy the changes to the appropriate device page Select a device in the tree control Page 40 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 15 Optional Enter the Retention Time for the selected device If you do not enter a time the entry appears in the initialization section of the PGM file 16 Specify the State or Duration e Clicking State in the tree control specifies a simple switch command Select Open or Closed from the drop down list box e Clicking a state description in the tree control sets the device to the selected state and lets you specify a Duration Enter the duration of the selected state in the edit box 17 To add the following information to the list box click Add e Retention Time value e Name of the selected Device e State or Duration value Chromeleon will automatically organize all entries in the list box in chronological order To remove an entry from the list box select the entry and click Delete All entries in the list box will automatically be reorganized 18 Click Next to continue The following screen is displayed Program Wizard Completion xi Completing the Program Wizard You now have entered all data required
9. On the File menu click Save Installation and then close the Server Configuration program 3 7 Installing the Flow Cell The detector is shipped without a flow cell Before initial operation of the detector install a flow cell that is appropriate for the respective application Flow cells must be ordered separately from Dionex Do not touch the cell windows If you touch a window clean it with isopropyl alcohol and a clean lens tissue NOTE No tools are required for removing and installing the flow cell The knurled head screws on the flow cell cover and tubing bracket can be loosened and tightened by hand Open the front panel door Remove the two knurled head screws on the flow cell cover and then remove the cover Fig 4 page 13 Analytical or semi micro cell Remove the two knurled head screws on the tubing bracket to remove the bracket from the lamp cover Fig 30 page 88 Squeeze the handle of the flow cell and insert it straight into the optical bench Release the handle and then pull it forward slightly If there is a click the cell is properly mounted If there is no click rotate the handle slightly just until the cell clicks into place Fig 14 Inserting the flow cell into the optical bench Operating Instructions Page 31 UltiMate 3000 Series Photodiode Array Detector 5 Thread the flow cell inlet tubing through the tubing guide on the lamp cover and reinstall the tubing bracket Fig
10. Spectrograph Lens Filter Paddle Slit Grating Photodiode Array Function 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 results over the selected wavelength range 2 4 Flow Cells All flow cells are optimized for fast separations with no loss in chromatographic resolution Note that the PDA is shipped without a flow cell Flow cells must be ordered separately from Dionex All cells are shipped with outlet fluidics backpressure line and capillary to the column compartment and fittings For information about how to install remove and clean flow cells refer to section 6 2 Do not touch the cell windows If yo
11. see page 49 e Bandwidth is too narrow Select a wider bandwidth and reference bandwidth if appropriate for the application For guidelines when selecting the sample and reference bandwidths see page 47 and page 49 e Front panel lamp cover or flow cell cover is missing Optical components are sensitive to temperature and light Do not operate the PDA 3000 unless the front panel lamp cover and flow cell cover are in place e Crimped or plugged tubing Over time tubings may become pinched off and plugged Periodically check all tubing and replace as needed section 6 1 page 83 e Flow cell installed incorrectly Check that the cell is inserted straight into the optical bench and is fully seated e Inappropriate rise time In general the rise time should be approximately 25 of the peak width at half height of the narrowest peak of interest See page 45 for more information e Detector exposed to high vibration Optical detectors are sensitive to vibrations Make sure the PDA 3000 installation site is vibration free e Filter paddle has malfunctioned If you have recently autozeroed the detector check the Audit Trail If the Filter wheel sensor could not detect blocked position or Filter wheel sensor could not detect open position message is displayed see page 65 for instructions Operating Instructions Page 73 UltiMate 3000 Series Photodiode Array Detector e Pump needs priming and or maintenan
12. 63 1 Lamp Diagnostics sense Ea re A narre eder DE 91 6 3 2 Replacing the Deuterium Lamp sssssssssssessessrsserssrsstssessreseesresressessersersressesne 92 6 3 3 Replacing the Tungsten Lamp GW u u u ssssusessersereeseenseenee renses erne sense r serne enee 95 6 4 Replacing the Main Power Fuses 97 Page ii Operating Instructions UltiMate 3000 Series Photodiode Array Detector 10 Specific tions eiccsscccscdescascssdaseraccesonssestocecaseevennesussicecnddenscesdeshodsoddesunnsesendecdenssounasssaatedses 99 Accessories Spare Parts and Consumables ses 101 8 1 1 Standard Accessories included in the Ship Kit 101 Sled Blow Cells ai sr RER in E E et dame ase 101 8 1 3 Spare Parts and Consumables 3255 oner i E EE 102 Technical Appendix Relay TTL Pin Assignment see 103 Index ins nn nus deacessesdagacsdeccousecsscedeepedsadeeseseasceatesseneccosesucenies 105 Operating Instructions Page iii UltiMate 3000 Series Photodiode Array Detector Page iv Operating Instructions UltiMate 3000 Series Photodiode Array Detector 1 Introduction 1 1 How to Use This Manual The layout of this manual is designed to provide quick reference to the sections of interest to the user However in order to obtain a full understanding of the detector Dionex recommends that you review the manual thoroughly before beginning operation NOTE The descriptions in this manu
13. Check the deuterium lamp intensity page 55 If the intensity reading is above 10 million counts for an analytical or semipreparative cell or above 3 million counts for a semi micro cell follow these steps a In Chromeleon press F8 to display the Commands dialog box b Select UV and UV_Calibration c Select Intensity and click Execute to calibrate the lamp intensity d Select Autozero in the Commands dialog box and click Execute to run the autozero routine e If no error message is displayed flush the cell with the mobile phase for the application and or clean the cell as instructed in Section 6 2 page 84 f Reinstall the cell in the optical bench Operating Instructions Page 75 UltiMate 3000 Series Photodiode Array Detector g Autozero the detector again to verify that the problem has been resolved If the problem remains contact Dionex Service for assistance If the intensity reading is below 10 million counts for an analytical or semipreparative cell or below 3 million counts for a semi micro cell follow these steps a Check that the flange of the deuterium lamp is aligned with the two locating pins in the optical bench Fig 35 page 93 If the flange is aligned the lamp is defective and should be replaced section 6 3 page 91 b If the intensity reading is still too low after the lamp was replaced contact Dionex Service for assistance e Filter paddle has malfunctioned Chec
14. Command on the Control menu NOTE For information about control commands also refer to the Chromeleon Online Help PDA 3000 Command Average Bandwidth BunchWidth Data_Collection_Rate NegativeAbsorptionLevel Offset_Level RefBandwidth RefWavelength Rise_Time Function When Average is On Chromeleon averages the data points between Step intervals gt page 53 Sets the bandwidth the wavelength range at which the chromatogram is measured of the sample wavelength page 48 Determines how many nanometers are averaged when collecting 3D data Bunching or averaging the signals of adjacent wavelengths reduces the size of the 3D data stored page 52 Sets the rate at which Chromeleon collects digital data points from the detector page 46 Adjusts the negative absorbance this permits the baseline and peaks to be seen even when the measured absorbance becomes negative after the Autozero page 54 Sets the offset applied to the recorder output Sets the bandwidth of the reference wavelength if one is selected If RefWavelength is Off the RefBandwidth setting has no effect gt page 50 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 page 48 Sets how quickly the detector responds to a change in signal page 45 Page 42 Operatin
15. Leaking fittings Locate the source of the leak Tighten or replace all liquid line connections 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 minutesto 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 Operating Instructions Page 71 UltiMate 3000 Series Photodiode Array Detector e 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 e Plot scale exaggerates baseline noise If autoscale is selected even a plot with low noise may fill the screen Check the Y axis scale values e Air bubbles in flow cell Remove the trapped air section 6 2 3 page 86 To prevent air from becoming trapped in the cell again follow these steps e Degas mobile phases and post column reagents by vacuum degassing or sparging with helium e Connect a backpressure line to the cell section
16. Series Photodiode Array Detector 4 3 Optimizing Detector Performance The performance of the PDA 3000 can be optimized by careful selection of key operating parameters This section defines these parameters describes how they interact with each other offers guidelines for their selection and includes example chromatograms The following table summarizes the topics discussed in this section Operating Parameter Performance Characteristics Affected Flow cell material Chemical compatibility Rise time Peak resolution sensitivity baseline noise Data collection rate Peak resolution disk space Sample wavelength Sensitivity linearity Bandwidth Sensitivity vs baseline noise Reference wavelength Baseline drift Reference bandwidth Baseline noise baseline drift Bunch width Spectral resolution peak match disk space Step Baseline noise rise time data collection rate disk space Average Rise time data collection rate Negative absorbance Peak detection baseline noise linearity Set automatically by Chromeleon Page 44 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 4 3 1 Flow Cell Material The flow cell materials must be chemically compatible with the mobile phases and analytes of interest Strong bases can etch the fused silica windows of the flow cell If the mobile phase is a base make sure the mobile phase concentration does not exceed 0 1 M Ifthe concentrat
17. and fittings and replace as necessary section 4 4 page 55 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 Operating Instructions Page 83 UltiMate 3000 Series Photodiode Array Detector Without the column backpressure is usually less than 0 34 MPa 50 psi depending on the flow rate and tubing ID Note that the semi micro flow cell will develop approximately 1 03 MPa 150 psi backpressure at 1 0 mL min If the backpressure remains high remove the fittings and tubing from part of the flow path section by section starting at the outlet connection work back upstream until you identify the section causing the substantial backpressure Replace tubing and fittings as necessary Periodically check the flow cell tubing connections for leaks or restrictions Replace tubing and fittings as necessary Periodically repassivate stainless steel systems This is especially important when operating with extreme pH levels which will shorten the life of the passivation finish or after a major disassembly Monitor baseline noise If the noise increases above an accepta
18. anoreksi id 44 Operating Instructions cceceeceeseeseeteeeeeeeeeeees 4 Operating Parameters 46 48 49 50 51 52 54 55 56 Operation Safety Precautions 6 Safety Symbols ccceccecseesseseeseeeeeeeeeeeseens 5 Optical Benchs sinistres 68 Optical System Components 16 TUUSIAtI on 2 4 ed ss eh ht 16 Page 106 Operating Instructions UltiMate 3000 Series Photodiode Array Detector P Parts Replacement cececeeseseeeeeeeeees 85 103 Passivation ioiii ae 86 PDA 3000 Applications 37 Peak Heights 11 544 tirant 47 Peak Identification 12 49 Peak Purityerssscen nines 10 12 49 Peak Resolution ccccecseeeseeeeeeeeeeeeeeeeeeeeeees 46 Peaks Asymmetrical 47 Co eluting rires nus 48 Improving height 81 Improving shape 82 Performance Optimization 46 48 49 50 51 52 54 55 56 Performance Optimization Time 47 PGM Files rarnana aan Et 39 80 PGM Wizard Sienen hie 39 Photodiode Array 10 16 17 Photodiode Array Detection 1 11 Pin Assignments Relay TTL 1 105 Post Column Reagents 74 81 Power Cord u u dsssseuesessrseseenssenseensrennee 30 99 Power LED ifs uns ananas Se 71 Power Switch 14 31 Power Up Diagnostic Test 57 Problems laser nd arr sn 61 Pumping System Requirements cc 23 R R ar Pan
19. application All mobile phase reservoirs should be compatible with the solvents used with your application Some plasticizers in blow molded components leach and are strong UV absorbers Cleanliness is very important After operating in detection modes that do not require optically clean reagents such as conductivity the solvent delivery system may need to be thoroughly cleaned A basic cleaning procedure is described below for additional information refer to the pump user s manual To avoid contamination always wear 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 en 9 ON SA Remove the column and the suppressor if installed Connect the line exiting the injection valve directly to the flow cell inlet tubing Flush the system with DI water at 1 0 mL min for 20 minutes Flush the system with methanol at 1 0 mL min for 20 minutes For very sensitive applications continue flushing for several hours Flush the system with DI water at 1 0 mL min for 15 to 20 minutes 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 DI water Refer to the pump user s manual for instructions Cleaning the pist
20. completed before attempting to issue any other command Command not executed because an Autozero command is already running To troubleshoot Wait until the autozero routine is completed before attempting to issue any other command Data is unavailable To troubleshoot This message appears if the PDA 3000 fails to respond when the computer attempts to communicate with the detector Shut down the Chromeleon server and turn off the PDA 3000 power wait 30 seconds and then power up both the server and the detector If the error message appears again contact Dionex Service for assistance amp Diagnostic is running To troubleshoot This message appears if you attempt to issue a command or select a parameter while a diagnostic routine is running Wait until the diagnostic routine is completed before making any changes Page 64 Operating Instructions UltiMate 3000 Series Photodiode Array Detector DSP communication failure To troubleshoot This message appears if there is a communication failure between the DSP digital signal processor and the CPU Turn off the PDA 3000 power for 30 seconds and then turn it on again If the error message appears again contact Dionex Service for assistance Filter wheel sensor could not detect blocked position D Filter wheel sensor could not detect open position A backup paddle alignment routine ensures that the PDA 3000 remains functional even if the sen
21. for 20 to 30 minutes at 1 0 mL min If the procedure above does not clean the cell follow these steps 1 Disconnect the liquid lines from the cell in and out connections 2 Connect a luer adapter to the cell in connection 3 Using a syringe flush the cell with a succession of at least 10 uL each of DI water acetone and 3 M HNO 4 Reconnect the cell liquid lines 5 Flush the cell with DI water for 20 to 30 minutes at 1 0 mL min 6 2 3 Removing Trapped Air from the Flow Cell Trapped air bubbles in the flow cell may cause pulsations of the baseline or random noise and low readings Flush the cell with methanol for 20 minutes If this does not remove the trapped air follow these steps 1 Disconnect the liquid line and or backpressure device from the cell out connection 2 Using a small syringe push 3 to 5 mL of methanol through the cell Or bypass the column and pump methanol through the system at 1 0 mL min 3 Reconnect the liquid line and or backpressure device Page 86 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 6 2 4 Replacing the Flow Cell The detector is shipped without a flow cell Before initial operation of the detector install a flow cell that is appropriate for the respective application NOTE No tools are required for removing and installing the flow cell cover and tubing bracket The knurled head screws can be loosened and tightened by hand Important Make
22. for Leakage After you have replaced the flow cell lenses and seals check the cell for indications for leakage 1 Connect the flow cell to the pump and install a backpressure capillary on the cell outlet Pressurize the flow cell as appropriate for the cell type The backpressure on the cell must not exceed the values specified in the table below Flow cell type Maximum backpressure PEEK analytical or semi micro cell 21 bar 300 psi SST analytical or semi micro cell 35 bar 500 psi Semipreparative cell 100 bar 1450 psi Inspect the flow cell for indications of leakage If there is any leakage tighten the retaining nut s with the windows replacement tool until the leak stops Dry the cell thoroughly with a lint free optical grade tissue Important Do not overtighten the retaining nut as this may fracture the window If tightening the retaining nut s does not stop the leakage remove the window and inspect the flow cell seal and groove for the cause of the leak If necessary clean the groove and reinstall the O ring section 6 2 5 page 89 Dry the cell thoroughly with a lint free optical grade tissue If the groove is scratched the cell must be replaced section 6 2 4 page 87 6 3 Lamps 6 3 1 Lamp Diagnostics Chromeleon includes a number of diagnostic functions for monitoring the wellness of your UltiMate 3000 chromatography system These functions help to prevent problems and ensure reliable ope
23. nm bandwidth and flowing water at 1 0 mL min lt 15 LAU at 520 nm 2 second rise time 10 nm bandwidth and flowing water at 1 0 mL min lt 1 mAU h at 254 nm and 520 nm and flowing water after warm up typically lt 500 pAU h 190 to 800 nm 1 nm self calibration with deuterium lines verification with built in holmium oxide filter lnm Corr Coeff gt 99 95 and lt 3 RSD up to 1 5 AU Stainless steel cell 13 uL volume 10 mm 0 394 in path length Stainless steel cell 3 1 uL volume 9 mm 0 35 in path length 0 7 uL volume 0 4 mm 0 02 in path length Analytical flow cell lt 21 bar 300 psi PEEK lt 35 bar 500 psi SST Semi micro flow cell lt 21 bar 300 psi PEEK lt 35 bar 500 psi SST Semipreparative flow cell lt 100 bar 1450 psi Single beam reverse optics design with concave holographic grating 1024 element 0 7 nm Operating Instructions Page 99 UltiMate 3000 Series Photodiode Array Detector Lamps Control GLP features Analog outputs Voltage out Power requirements Fuses Dimensions h x w x d Environmental conditions Weight Decibel level Deuterium lamp 30 W for ultraviolet spectrum analysis Tungsten lamp 15 W for visible spectrum analysis All parameters and functions controlled by Chromeleon software the Chromeleon PC and the detector are connected through USB Universal Serial Bus
24. output and offset within the 0 to 1 volt range The analog outputs continue to output data even after the computer running Chromeleon is turned off or is disconnected from the PDA 3000 When the detector power is turned on again the analog output settings will be either the factory defaults section 4 4 page 55 or the settings selected the last time the detector was controlled by the computer Operating Instructions Page 27 UltiMate 3000 Series Photodiode Array Detector 3 5 3 Relay TTL Connections The two TTL outputs and two Relay outputs on the instrument s rear panel Fig 9 page 19 can be used in Chromeleon to exchange digital signals with external instruments The accessories kit includes a 12 pin connector part no 6080 9010 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 the small screwdriver included in the ait The TTL and Relay outputs can be programmed as part of a PGM file section 4 2 2 page 37 in Chromeleon or controlled manually through a Control panel in the software For information about the port and pin assignment refer to the technical appendix page 103 A Caution Connection of relay loads and their power sources to the TTL outputs will damage the TTL output stage If the relay load can source more than 200 mA at 5V or higher it may damage the Data Processing board A Warn
25. plupart des solvants organiques il a tendance gonfler lorsqu il est en contact prolong avec du chloroforme CHCH du dim thyle sulfoxyde DMSO ou du t trahydrofurane THF De plus il est attaqu par des acides concentr s tels que l acide sulfurique et l acide nitrique ou d un compos du hexane thyle ac tate et m thanol Ces acides peuvent cependant tre utilis s dans le cadre de proc dures de nettoyage condition que l exposition soit br ve e N utilisez pas de tubes PEEK cras s pli s ou abim s e Au cours du fonctionnement la lampe et les pi ces qui l entourent deviennent extr mement chaudes et le restent pendant quelques temps apr s que le d tecteur ait t arr t A fin d viter de possibles br lures laissez la lampe refroidir pendant une p riode suffisamment longue avant de proc der tous travaux de maintenance ou de r paration e La lampe au deut rium met des rayons UV qui sont dangereux pour les yeux Par cons quent vitez de regarder directement la source de lumi re et portez des lunettes de protection Arr tez toujours le d tecteur avant de remplacer la lampe e Utilisez des pi ces de rechange d origine Dionex Effectuer des remplacements par des pi ces ne provenant pas de Dionex ou utiliser des accessoires ne provenant pas de Dionex peut affecter les performances de l instrument e N utilisez pas l instrument de mani re autre que celles d crites dans ce manuel Page 6 O
26. solvent rack to the pump and from the pump to the detector as shown in Fig 18 a Dionex recommends connecting the drain tubing from the column compartment as shown in Fig 18 b This is to avoid that the gas sensor in the column compartment is influenced by the drain tubing from the other modules As an alternative you may direct the drain tubing from the Tee of the column compartment separately to the waste container Connect the drain tubing from the detector as shown in Fig 18 c Dionex recommends cutting the tubing which is provided in the instrument s accessories kit to the following lengths Tubing from Length mm Solvent rack to pump 215 Pump to detector 332 Page 34 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 4 Detector Control The PDA 3000 Photodiode Array Detector is designed for use with IC ion chromatography BioLC biocompatible liquid chromatography and HPLC high performance liquid chromatography systems and should not be used for any other purpose Operation of the PDA 3000 in a manner not specified by Dionex may result in personal injury If you have a question regarding appropriate usage contact Dionex Service before proceeding 4 1 Getting Started Before beginning operation of the PDA 3000 follow these steps 1 Press the Power switch on the front panel to turn on the detector Fig 3 page 11 2 Verify that the Power LED is lighted 3 Verify that the Deuteri
27. to create the program Please enter a title describing your program PD4 3000 Manual Now you can either save the program to disk immediately or review it and save it later C Save the program immediately Review the program in a new window Press Finish to open the program in a new window lt Back Cancel Hep Fig 24 Program Wizard Finishing the program 19 Optional Type a descriptive Title for the program 20 Select one of the following options Operating Instructions Page 41 UltiMate 3000 Series Photodiode Array Detector e To save the programm without first reviewing it select Save the program immediately Clicking Finish opens a dialog box in which you can save the program e To review the program before saving it select Review the program in a new window Clicking Finish opens the program in the PGM Editor Use the PGM Editor to review the program and to manually edit it if necessary When you finish exit the PGM Editor This displays a prompt asking whether the program should be saved clicking Yes opens a dialog box in which you can save the program 4 2 3 Control Commands Chromeleon includes many control commands that are available for all detectors In addition there are commands that are exclusively for the PDA 3000 see the table below These commands can be selected from either the default Control panel or the Commands dialog box To open the Commands dialog box press F8 or select
28. to the cell out connection Important Make sure not to twist the end of the flow cell inlet and outlet tubings when connecting them from to the liquid line connections Preferably use a tool to hold the union fitting while you remove or install any connections Fig 16 Union fitting 9 The detector enclosure provides four slots Fig 4 page 13 Thread the lines connected to the flow cell in and out connections through these slots to prevent them from being pinched when the front panel door is closed 10 Close the front panel door 11 Connect the cell inlet connection to the separator column outlet 3 8 Connecting the Waste Tubing Connect the waste tubing part no 6000 5001 to the outlet at the bottom right see figure below Place the free end of the waste tubing in a waste container below the level of the workbench on which the PDA 3000 is installed Outlet at the bottom right of the detector Abb 17 Outlet Important The tube must remain below the drain port If the tube is above the drain port the drip tray may overflow inside the detector Operating Instructions Page 33 UltiMate 3000 Series Photodiode Array Detector If the detector is part of an UltiMate 3000 system you may connect the drain tubing of the system modules with the connecting pieces from the devices accessories kits Connecting 7 i a b Fig 18 Connected drain tubing Connect the drain tubing from the
29. utiliser de branchement mis la terre VAN Mise en garde 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 Connect a modular power cord IEC 320 C13 from the PDA 3000 main power receptacle Fig 9 page 19 to a grounded single phase power source Use the front panel Power switch to turn the detector on and off 3 6 Setting Up the Detector in Chromeleon This section provides brief instructions for setting up Chromeleon For details about any of these steps refer to the Chromeleon Help NOTE Dionex recommends installing the Chromeleon software before connecting the detector to the USB port on the Chromeleon computer When you install the Chromeleon software first the Windows operating system will detect the detector automatically when the detector power is turned on 3 6 1 Loading the USB Driver for the Detector 1 Turn on the computer power if it is not already on 2 If this is a local computer log on to the Windows operating system XP or 2000 as a local administrator If this is a network computer log on as a user with local computer administrator privileges 3 Start the Chromeleon Server Monitor program by double clicking the Chromeleon Server Monitor icon Sa on the Windows taskbar If the Server Monitor icon is not on the taskbar click Start on the taskbar point to Progr
30. 00 0 0100 1 i i i mi 0 00 1 00 2 00 3 00 4 00 5 00 Rise Time 2 0 sec Baseline Noise 10 AU 0 0150 MAU WVL 254 nm 0 0000 0 0100 0 0200 iz 0 00 1 00 2 00 3 00 4 00 5 00 Fig 25 Effect of Rise Time on Baseline Noise 4 3 3 Data Collection Rate The data collection rate or sample rate is the number of data points per second Hz at which the computer stores data from the PDA 3000 The detector electronics always collect data at up to 20 0 Hz The data collection rate settings are 0 25 0 5 1 0 2 0 2 5 default 5 0 10 0 Hz or 20 0 Hz The maximum number of data points is stored at 20 0 Hz Slower data collection rates store the average of the 10 0 Hz points for example a 5 Hz rate stores the average of four 20 0 Hz points e In general each peak should be defined by at least 20 data points For chromatograms with co eluting peaks or low signal to noise ratios 40 data points per peak is recommended e Ifall peaks are relatively wide select a slower data collection rate 1 0 Hz for example e If any peaks of interest are less than a few seconds select a faster data collection rate 5 0 Hz for example Page 46 Operating Instructions UltiMate 3000 Series Photodiode Array Detector e Ifthe data collection rate is too slow the start and end points of peaks are not accurately determined If the collection rate is too fast data files may occupy excessive disk space an
31. 000 272 10 I UV VIS 4 0 000 30 000 520 10 5 M UV VIS 5 0 000 30 000 600 10 l6 m 3DFIELD RefWavel nm Oo 3D Min Wavelength E 190 790 nm 3D Bunchwidth 2 1 25 nm 80 3D Max Wavelength 0 200 800 nm lt Back Cancel Help Fig 22 Program Wizard UV Options Enter the Data Collection Rate and the Rise Time NOTE NOTE When the data collection rate is set to 10 0 Hz the 0 05 second rise time setting is not available When the data collection rate is set to 20 0 Hz the 5 0 second rise time setting is not available The 20 0 Hz data collection rate and 0 05 second rise time settings are not supported unless PDA 3000 Firmware version 1 1 0 or later is installed To program UV VIS 1 through UV VIS 5 the single wavelength channels a Check or clear a check box to determine whether 2D data from this channel will be collected b For each selected channel enter the starting and ending data acquisition times as well as the wavelength bandwidth reference wavelength and reference bandwidth NOTE NOTE The settings for these channels apply to both analog outputs and ditigal outputs UV channel 1 analog output UV2 analog output 2 etc When the reference wavelength is off the reference bandwidth is not used The reference value is the first data point of the sample wavelength and bandwidth after autozero Operating Instruct
32. 3 6 page 29 This increases the backpressure on the cell thereby shrinking bubbles and allowing them to pass more easily through the cell e Contaminants in flow cell Clean the cell section 6 2 page 84 e Incorrect lamp selected If a UV wavelength is selected make sure the deuterium lamp is on If a visible wavelength is selected make sure the tungsten lamp is on When a lamp is on the corresponding front panel LED Deuterium or Tungsten is lighted e Lamp needs replacement The light output of the lamp decreases over time The lower light output may increase noise above an acceptable level especially if the lamp has been in service for more than 2000 hours If this occurs replace the lamp See Section 6 3 page 91 or Section 1 page 92 for instructions on replacing the deuterium lamp or tungsten lamp respectively e Lamp incorrectly installed Make sure that both lamps are fully seated in the optical bench See Section 6 3 page 91 or Section 1 page 92 for installation instructions for the deuterium lamp or tungsten lamp respectively Page 72 Operating Instructions UltiMate 3000 Series Photodiode Array Detector e Inappropriate reference wavelength Select a reference wavelength in a quiet area of the spectrum where little absorption occurs Dionex recommends selecting a reference wavelength below 380 nm for UV applications and above 600 nm for visible applications For more information
33. 3000 Series Photodiode Array Detector 5 11 Low Spectral Resolution Bunch width too wide Select a bunch width setting of 1 nm and then check the resolution again 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 bandwidth 5 12 Peaks Too Large or Small Analog data collection Check the recorder and integrator input voltage The PDA 3000 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 page 45 and data collection rate page 46 are appropriate to capture the narrowest peak Prepare fresh post column reagent Verify that the reagent flow rate is correct Reference bandwidth too wide Select a narrower reference bandwidth The reference bandwidth should not overlap the sample bandwidth Operating Instructions Page 79 UltiMate 3000 Series Photodiode Array Detector 5 13 Poor Peak Sha
34. 4 LEDs Power Run Deuterium Tungsten for status monitoring In Chromeleon Support of automatic equipment qualification AutoQ and System Wellness monitoring All system parameters are logged in the audit trail Four 0 3 AU independently selectable 1000 mV range 1 V output 85 to 265 VAC 47 to 63 Hz auto sensing no adjustment necessary Typical input power 100 W Maximun line draw 3 5 A at 110 VAC at power up Two 4 0 amp fast blow IEC 127 fuses Range of use Indoor use Temperature 10 to 35 C 50 to 95 F Air humidity 80 relative humidity non condensing Overvoltage category II Pollution degree 2 19 x 42 x 51 cm 7 5 x 16 5 x 20 in 19 kg 41 8 Ibs lt 50 dbA during routine operation 56 dbA at power up Page 100 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 8 Accessories Spare Parts and Consumables Accessories spare parts and consumables for the detector are always maintained at the latest technical standard Therefore part numbers are subject to alteration However updated parts will always be compatible with the parts they replace 8 1 1 Standard Accessories included in the Ship Kit The following accessories are shipped with the detector The list is subject to change without notice Some parts listed below are included in one of the spare part kits For information about these kits refer to section 8 1 3 page 102 pese kit S
35. 8 Deuterium Lamp 94 Flow Gell 3 SAREEN eener 86 Fuse Replacement 99 Lapi ste tant eines 93 Removing trapped air from cell 88 Tungsten Lamp Replacement 1 97 Shutdown Procedure 85 Signal Intensity Slit optical ss Source LENS sscscessiscsesesescgstetaisesessseibesianvesaseneescas Spare Parts Spectra not collected 80 Spectral Library Spectrograph Lens SPECITUM 6 men tem Mt essuie Spectrum Improving Resolution Guidelines for Selecting Selection by Software System Wellness Technical Support Temperature ambient Timebase sayisi Troubleshooting Baseline Drift Baseline Noise Diagnostic Tests ccccecceceescesseeeeeeeseeneeees Elution time is slow Filter Paddle Malfunction 00 Lamp does not light Lamp Intensity eee PDA 3000 does not respond Peak shape is poor ccecccecceeseeeseeereeeeeeees Operating Instructions UltiMate 3000 Series Photodiode Array Detector Peak size is Wrong 81 USB nt At en rien 10 28 Spectra not collected 80 Configuration File u seveserererereee 73 83 Spectral resolution is poot ss cc 81 Connection to Hub 28 USB communication problem 83 USB Cable sense es tes te 28 Wavelength calibration fails 1 78 USB Communication Problem s s s1sss1s0seeee 83 Wave
36. AURE Enr coh des rime or terne Intensity Lamp does not light 72 On Off Control sardiner 45 Output Waning u sssceeeserrerererererre renee 74 Replacing seen tn et lens 94 Time to Stabilize 37 73 76 Deuterium LED sal ls 72573 DIA STIOSTICS ed menti rte in 93 Disk Space sites ans nes 46 49 DE ii tiie Need een de 35 Drain Tube 35 105 UltiMate 3000 Series Photodiode Array Detector E Electronics 3 sai eosin hela ee 85 F FAN SRE rene res Re 68 Ferrule Fittings ccccssssscseseeresssssseeceseeensens 73 Filter Paddle Flashing LED inner 71 Flow Cs ses see nr hrs he 17 Air BUDDIES ssnin hahae 88 Chemical Compatibility 00 0 ee 17 47 Cleaning RES ERE SEES nent tie 88 Installation 0 0 cccccccccscsccceesseeccessseeeeseesees 33 Leakage Checkpoint es 93 TIC AKS innn e rnu E nee 87 Maintenance 86 Material asst onion eet ah oe 47 Replacement 353 usine 89 Windows and Seals Replacement 91 Found New Hardware Wizard 32 Front Panel nana Rice 15 Front Panel LEDs 13 Eus Holder screams danaa nes ren tn 99 USCSES NRA E GENET te ent nl ee 99 G Gradient Analyses 77 Gradient Applications Gradient Elution 23 Negative Absorbance W Wu u ssseseererserrrnneee 56 Reference Wavelength Selection 51 Grating optical cceeeeseeeeeeeeeeeeeeeeees 16 17 H
37. Cell Heat Exchangers L Spring Clip Fig 7 Semi Micro Flow Cell Assembly Description PEEK P N Stainless Steel Flow Cell P N Reducing union fittings 6080 2102 Cell outlet tubing 6080 2403 0 25 mm 0 010 in ID Outlet fluidics kit including 6080 2411 capillary with tubing and fitting Operating Instructions Page 17 UltiMate 3000 Series Photodiode Array Detector Semipreparative Flow Cell Part No 6080 0240 Cell Cell Cell Path Volume of Heat Intended Flow Material Volume Length Exchanger Inlet Rate Range Tubing PEEK 0 7 pL 0 4 mm N A 5 to 100 0 mL min The semipreparative flow cell assembly Fig 8 is available in PEEK only The cell is desinged for use with semipreparative flow applications and flow rates of 5 0 to 100 0 mL min The 0 4 mm path length minimizes detector absorbance for concentrated peaks Cell Outlet Tubing OR 0 51 mm 0 020 in ID U Fitt nion Fitting SS a Se Handle ag Nay Spring Clip i y Cell Inlet Tubing Pa bs 0 51 mm 0 020 in ID Union Fitting Flow Cell Fig 8 Semipreparative Flow Cell Assembly Description PEEK P N 6080 0240 Union fittings 6080 2103 Cell inlet or outlet tubing 6080 2406 0 51 mm 0 020 in ID Outlet fluidics kit including 6080 2412 capillary with tubing and fitting Page 18 Operating Instructions UltiMat
38. Dionex Shipping insurance will compensate for the damage only if reported immediately Keep the original shipping container and packing material They provide excellent protection for the instrument in case of future transit Shipping the unit in any other packaging automatically voids the product warranty Place the shipping container on the floor and remove the accessories Grasp the detector by the sides Slowly and carefully pull the instrument out of the shipping container and place it on a stable surface To prevent the detector from falling always lift the unit by the sides Do not lift the detector by the packing material or the front panel door Afin d emp cher l instrument de tomber saisissez la par les c t s Ne soulevez l instrument l aide du mat riau d emballage ou par la porte du panneau avant Operating Instructions Page 23 UltiMate 3000 Series Photodiode Array Detector 3 Before connecting the detector to the power supply wait approximately 1 hour to allow the instrument to come to room temperature and to allow any condensation that might have occurred during shipping to evaporate After 4 hours check the detector if condensation still exists allow the detector to continue to warm up without connecting it to the power source until the condensation is completely gone 3 3 Positioning the Detector in the UltiMate 3000 System If the detector is part of an UltiMate 3000 system e g for analyti
39. E All repairs of the PDA 3000 electronics must be performed by qualified Dionex Service personnel Before replacing any parts review the troubleshooting information in Chapter 5 gt page 59 to isolate the cause of the problem Substituting non Dionex parts may impair the performance of the PDA 3000 thereby voiding the product warranty Refer to the warranty statement in the terms of sale for more information Before you return any instrument to Dionex for repair contact Dionex Service or your local distributor An RMA number Return Material Authorization number is required in order to track your instrument Always use the original packaging and observe the packing instructions Service Return Form section in this manual binder when shipping the PDA 3000 Shipping the instrument in anything other than the original packaging will void the warranty Refer to the warranty statement in the terms of sale for more information 6 1 Regular Maintenance Procedures e Before shutting down the detector for more than 24 hours flush the system with deionized DI 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 e Periodically check the waste line connected to the leak tray at the bottom of the optical bench Verify that the tubing is unclogged and that it is routed below the leak tray e Periodically check all tubing
40. ED is no longer flashing resume normal operation If the reading is acceptable but the Power LED is still flashing contact Dionex Service for assistance If the reading is too low follow the troubleshooting steps in section 5 7 page 75 5 3 Lamp Does Not Light or Lamp LED Is Flashing Lamp default setting is not in effect When the factory default settings are in effect the deuterium and tungsten lamps turn on automatically each time the detector power is turned on If the required lamp does not turn on automatically you can turn it on from Chromeleon or from the TTL input To restore the default setting for a lamp 1 Press F8 in Chromeleon to display the Commands dialog box and select UV 2 Select UVLampPowerOnSetting for the deuterium lamp and click Execute 3 Select VisLampPowerOnSetting for the tungsten lamp and click Execute Lamp is old or burned out Replace the lamp See section 6 3 page 91 or section 1 page 92 for instructions on replacing the deuterium lamp or tungsten lamp respectively 5 4 No Detector Response Detector power not on Check that the power cord is connected from the PDA 3000 rear panel to a power source Check that the main Power switch is turned on Check the fuses and replace them if necessary section 6 4 page 95 Lamp not turned on Turn on the lamp from either Chromeleon or the TTL input When a lamp is on the corresponding front panel LED Deuterium or Tungsten
41. Heat Exchanger Volume s sesseeseeeee 18 19 20 Heat Exchangers cccceseesseeeeeeeeeeseees 18 19 Holmium Oxide Filter 10 17 Hubs USB uni ue a en ie 28 I Inside Front Panel 15 Installation Flow Cell saines PRR nas in Chromeleon Rear Panel Connections sssccerrree 28 Rev TL arenaer 105 Site Requirements 25 Software ss nn oe ait kates 28 UltiMate 3000 System cceceseeeeeereeees 26 Waste Tubing Inte Stator A ss ee a en an ee Intensity Lamp Isocratic Analyses Lamp Connections 95 Lamp Diagnostics 93 Lamp Intensity Replacement Leak S nSor ane rue ON oewts cae Leak Sensor Error 68 Leak Tay an ea a nef 85 Leaks Flow Cell missini Leak Sensor 1 Leak Sensor Error Symptoms LED Flashing sun siens L NSES eee RAN teens Pen Re ess Liquid Lines Maintenance 85 86 87 Maintenances uren haces 85 Mobile Phases Concentration Guidelines Degassing ieren Lamp Stability after Changing Pr parations ile in es Ent Reservoir Material Retention Time ccccccesccesseceesseeeneeeene Solvent Quality Temperature Stabilization 18 19 N Negative Absorbance ceeee 44 46 56 76 Normal Phase Solvents 17 NOTES in manual 6 Offset Level
42. L connection 6080 9020 Union fitting for semipreparative flow cell 6080 2103 USB cable type A to type B USB 2 0 5m 6911 0002 Waste fluidics kit including 6000 5001 2 m tubing 5 Tee pieces The part number always refers to the packing unit For more information please contact your Dionex sales representative Page 102 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 9 Technical Appendix Relay TTL Pin Assignment RELAY OUT TTL TTL IN TTL OUT GND 1 2 1 211 2 3 4 1 2 1 2 34 5 6 7 8 9 101112 Fig 38 Relay and TTL Connector The table below describes the pin assignments for the Relay and TTL connectors Relays 1 and 2 can be configured in Chromeleon to switch any low voltage control The switched current must be less than 200 mA and 42 V peak Pin Assignment Input Pin Function 1 Relay 1 output Active 2 Relay 1 output Ground 3 Relay 2 output Active 4 Relay 2 output Ground 5 TTL 1 output Active 6 TTL 2 output Active 7 TTL 1 input Active Autozero 8 TTL 2 input Active erna TEGIN 9 TTL 3 input Active UV lamp on off 10 TTL 4 input Active Visible lamp on off 11 TTL input or output Ground 1 12 TTL input or output Ground 2 Fig 39 Relay and TTL Pin Assignment Operating Instructions Page 103 UltiMate 3000 Series Photodiode Array Detector Page 104 Operating Instructions UltiMate 3000 Series Photodiode A
43. M mh hae W Yan h A Mal I M Vy Nw A A V Il A VVA N v V VI w i M mr ENT Wy im U l V We A JL Pj Bandwidth 4 yi t amia y na UW Noise 16 AU M ame Mit lo UN Ale nA IL A af aoe VA PMU ll healt AL UNI Wy RAS INN IN ul n AN LA A IAWN HAL JM 1 ny H IL Bandwidth 1 y li ami AL We E VE Ii ry Wl Wl Noise 26 pau IR TW We Wy I j ie T T T T T T Fig 26 Effect of Bandwidth on Baseline Noise Page 48 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 4 3 6 Reference Wavelength The reference wavelength is the center wavelength of the reference intensity determination Absorbance is measured by comparing the reference intensity to the sample intensity Selecting a reference wavelength implies a reference mode for each of the single wavelengths being collected There are two types of reference mode active or off e To select the active reference mode enter a wavelength within the selected sample scanning range of the PDA 3000 The selected wavelength will be used as the reference wavelength The reference intensity will vary over time as the signal intensity changes For maximum compensation select a reference wavelength from the same lamp as the sample wavelength For example e Ifthe sample wavelength is 272 nm you might select a reference wavelength of 325 nm because both wa
44. Now sold under the Thermo Scientific brand Thermo SCIENTIFIC Part of Thermo Fisher Scientific UltiMate 3000 Series Photodiode Array Detector Operating Instructions vowel NLL Revision 1 1 Date October 2007 2007 Dionex UltiMate 3000 Series Photodiode Array Detector Operating Instructions EZ DIONEX CE Declaration of Conformity Product Detector Type PDA 3000 Dionex Softron GmbH herewith declares conformity of the above products with the respective requirements of the following regulations e Low Voltage Equipment Directive 73 23 EEC changed by 93 68 EEC e EMC Directive 2004 108 EG The electrical safety of the products was evaluated based on the following standard e EN 61010 1 2002 Safety requirements for electrical equipment for measurement control and laboratory use Part 1 General Requirements The Electromagnetic Compatibility EMC of the products was evaluated based on the following standard e DIN EN 61326 2004 Electrical equipment for measurement control and laboratory use EMC Requirements This declaration is issued for the manufacturer Dionex Softron GmbH Dornierstrasse 4 D 82110 Germering by the President Dr Peter Jochum August 1 2007 Dr Peter Jochum Operating Instructions Page I UltiMate 3000 Series Photodiode Array Detector Certificate TUV License Holder Manufacturing Plant Dionex Corporation Dionex Corporation 541 Lake
45. Open the UltiMate 3000 PDA 3000 pan control panel 4 Click the Diagnostics button The PDA 3000 diagnostics panel opens Click the wavelength script button under Calibration The detector will perform the wavelength calibration routine and upload the result pass or fail to Chromeleon If the wavelength calibration fails follow the steps in Section 5 8 gt page 76 to resolve the problem Page 56 Operating Instructions UltiMate 3000 Series Photodiode Array Detector e Wavelength verification Purpose Tests the accuracy of the selected wavelength The result of the last wavelength verification test is stored in the calibration log and can be retrieved at any time Run the wavelength verification test for both the deuterium and tungsten lamps approximately every 6 months 1 Inthe Browser navigate to the following folder Dionex Templates Panels Dionex_LC 2 Open the UltiMate_3000_PDA 3000 pan control panel 3 Click the Diagnostics button The PDA 3000 diagnostics panel opens Click the wavelength verification script button under Diagnostic Tests The detector will perform the wavelength verification test and upload the result pass or fail to Chromeleon If the wavelength verification fails calibrate the wavelength and then run the wavelength verification test again If the lamp fails again follow the steps in Section 5 9 page 78 to resolve the problem NOTE After you have performed instrument qualificatio
46. SB port on the computer running Chromeleon NOTE Apart from the solvent rack all modules of the UltiMate 3000 system can be connected separately to the server PC However Dionex recommends interconnecting all modules and then connecting the system to the Chromeleon server PC via only one connection To do so use the USB hub on the pump or autosampler 1 Plug the A connector of a USB cable into the USB port on the computer Fig 12 2 Plug the B connector of the USB cable into a USB receptacle on the PDA 3000 rear panel USB Cable PDA 3000 Plug the USB cable s B 9 connector into the USB a receptacle on the PDA 3000 Plug the USB cable s A connector into the USB port on the PC Fig 12 PDA 3000 Connected Directly to the Chromeleon PC If a USB port is not available on the PC connect the PDA 3000 to an external USB hub and then connect the hub to the PC The hub and extra USB cable required for this configuration are options and are not included with the PDA 3000 Page 26 Operating Instructions UltiMate 3000 Series Photodiode Array Detector The USB standard limits the USB cable length to 5 meters 5 5 yds Each USB device can be separated from the PC by no more than five hubs Thus if five hubs are installed each USB device can be located no more than 30 meters 32 yds from the PC Carefully secure all USB cables the USB hub and the hub power cable so that they cannot
47. ach TTL input controls during stand alone operation TTL Input PDA 3000 Parameter TTL 1 in Autozero TTL 2 in Reserved TTL3 in Deuterium lamp on off TTL 4 in Tungsten lamp on off Page 58 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 5 Troubleshooting The following features help you to identify and eliminate the source for problems that may occur during the operation of the detector or an UltiMate 3000 system Error Messages If a fault or mechanical error is detected during the operation of the detector an error message is displayed in the Chromeleon Audit Trail Section 5 1 gt page 60 describes error messages and how to troubleshoot them Status Indicators The status indicators on the front panel display provide a quick visual check of the operational status of the detector For troubleshooting information when an LED is flashing refer to section 5 2 gt page 69 Operating Problems Section 5 2 page 69 through Section 5 14 page 81 describe routine operating problems and how to resolve them Diagnostics Tests If the detector is connected in Chromeleon Chromeleon provides several diagnostic tests allowing you to check the performance of certain detector components For more information refer to Section 4 4 page 55 If you are unable to eliminate a problem following the instructions given here contact Dionex Service Op
48. al refer to firmware version 2 0 and Chromeleon 6 80 Service Pack 2 The term the detector or the PDA is used throughout the manual The information contained in this manual is subject to change without notice and should not be construed as a commitment by Dionex Dionex assumes no responsibility for any errors that may appear in this document This document is believed to be complete and accurate at the time of publication In no event shall Dionex be liable for incidental or consequential damages in connection with or arising from the use of this document CHROMELEONP is a registered trademark of Dionex UltiMate is a trademark of Dionex All other trade or company names mentioned are subject to the copyright and the property and trademark rights of the respective companies All rights reserved including those for photomechanical reproduction and storage on electronic media 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 Operating Instructions Page UltiMate 3000 Series Photodiode Array Detector 1 2 Safety Information The CE Mark label and the cTUVus Mark safety label on the instrument indicate that the instrument is in compliance with the rela
49. ameters are NOT VALID Wavelength 190 to 600 nm Reference wavelength 750 nm Reference bandwidth 50 nm These parameters are invalid because 750 nm 25 nm 50 of 50 nm 775 nm which is greater than 600 nm When the data collection rate is 20 Hz select parameters that meet the following criteria Minimum lt 2 gt lt Maximum Maximum Minimum lt 310nm Where Reference wavelength BW Reference bandwidth For example the following parameters are VALID Wavelength 190 to 500 nm Reference wavelength 450 nm Reference bandwidth 50 nm These parameters are valid because 190 to 500 nm is a range of lt 310 nm and 450 nm 25 nm 50 of 50 nm 475 nm which is less than 500 nm Page 62 Operating Instructions UltiMate 3000 Series Photodiode Array Detector The following parameters are NOT VALID Wavelength 190 to 600 nm Reference wavelength 750 nm Reference bandwidth 50 nm These parameters are invalid because 190 to 600 nm is a range of more than 310 nm also 750 nm 25 nm 50 of 50 nm 775 nm which is greater than 600 nm Acquisition On for 3DFIELD rejected no 3D Data Acquisition license found To troubleshoot Chromeleon cannot perform digital data acquisition of a 3D data field unless the software includes the 3D Data Acquisiton license Contact Dionex if you want to order this option A Autozero is already in progress To troubleshoot This messa
50. amp Does Not Light or Lamp LED Is Flashing ccceeccessseeseeesseeseeesseeees 70 5 4 No Detector Response nd errant entiere rfi dde 70 5 5 Noisy Baseline sn enn aa n rr item ren 71 5 6 Drifting Baseline 22e armee mienne inerte 74 5 7 Deuterium Lamp Intensity Reading Too Low 75 5 8 Wavelength Calibration Fai ls 76 5 9 Wavelength Verification Fails c ccccccesccesceeececeeceeeeeeneceaeceeeesneeeaeeeeeeseeeeaeens 78 5 10 No Sp tra Coll cted see n E EN R T a NA at 78 5 11 Low Spectral Resolution 79 5 127 Peaks Too Large or Small tn nn edges at td et nn 79 5 13 Poog Peak Shapers aa rr et rn tirent durer tee 80 5 14 Faulty USB Communication 81 6 Routine Maintenance scccccssscsssccsscccsscssscssssccsscssssssssssscsscosssossscsssssssssssscsssoons 83 6 1 Regular Maintenance Procedures 83 6 2 Flow CIE ste eet iene eae dae ee eee 84 CAR Liquid Leaks Aso tr etic ene lens etree M nn at nt id 85 62 2 Cleaning th Flow Cela sein daa iaee eaten des nest 86 6 2 3 Removing Trapped Air from the Flow Cell 86 6 2 4 Replacing the Flow Cell 87 6 2 5 Replacing the Flow Cell Windows and Seals 0 ccceesssccssteeeetseeesteeeeseeeenes 89 6 2 6 Checking the Flow Cell for Leakage ccc cccccecessceesneeeeneceeseeenseeesseeenees 91 6 3 LaMpS sr Nr de EDER Ten Se REE re bead 91
51. ams or All Programs depending on the operating system point to Chromeleon and then click Server Monitor 4 Click Start to start the server Si wt 5 Click Close to close the Server Monitor window The Server Monitor icon on the taskbar appears NOTE Clicking the Quit Monitor button quits exits the Server Monitor program but does not stop the server To stop the server click Stop 6 Turn on the power of the detector Operating Instructions Page 29 UltiMate 3000 Series Photodiode Array Detector Microsoft Windows will automatically detect the new detector and launch the Found New Hardware Wizard which guides you through the USB installation Select the following options a Accept the default option Install the software automatically and click Next gt b Click Finish when the wizard reports that the software for the detector has been installed If Windows fails to detect the detector and a message box asks for a USB configuration file cmwdmusb inf this indicates that you connected the detector to the computer and turned on the power for the first time before you installed Chromeleon To resolve the problem a Click Cancel in the Windows message box b Turn off the detector and unplug the USB cable from the computer c Install Chromeleon d Reconnect the USB cable to the computer and turn on the power to the detector Windows will now automatically detect the detector and laun
52. be accidentally disconnected Plug the A connector of a USB cable provided in the PDA 3000 Ship Kit into a port on the external USB hub Plug the B connector of the cable into the USB receptacle on the PDA 3000 rear panel Fig 13 2 Plug the A connector of a standard USB cable into a USB port on the computer Plug the B connector of the cable into the B port on the USB hub Fig 13 USB Device USB Device USB Cables PDA 3000 Plug the USB cable s B connector into the USB receptacle on the PDA 100 Plug the USB cable s A connector into the A port on the USB hub Chromeleon Computer Plug the USB cable s A connector into the USB port on the PC Plug the USB cable s B connector into the B port on the USB hub Fig 13 Three USB Devices Connected to a USB Hub 3 5 2 Analog Output Connection Connect a recorder an integrator or an A D data acquisition device to the ANALOG OUT connector on the PDA 3000 rear panel Fig 9 page 19 The four PDA 3000 analog outputs are standard female BNC connectors and provide a 1 volt output maximum The full scale absorbance range can be set to 0 0005 0 001 0 01 0 1 0 5 1 0 2 0 or 3 0 AU full scale in Chromeleon The outputs are controlled by absorbance wavelengths 1 through 4 in Chromeleon The software controls the wavelength sample bandwidth reference wavelength full scale absorbance
53. ble level especially after a lamp s has been in service for an extended length of time replace the lamp section 6 3 page 91 Use the diagnostic functions in Chromeleon to check the lamp lifetime intensity and wavelength calibration section 4 4 page 55 6 2 Flow Cell The table below lists the flow cells available for use with the PDA 3000 All cells are shipped with outlet fluidics backpressure line and capillary to the column compartment and fittings Description Part No Analytical flow cell cell volume 13 ul cell material PEEK 6080 0200 Analytical flow cell cell volume 13 ul cell material steel 6080 0210 Semi micro flow cell cell volume 3 1 ul cell material PEEK 6080 0220 Semi micro flow cell cell volume 3 1 ul cell material steel 6080 0230 Semi preparative flow cell cell volume 0 7 ul cell material PEEK 6080 0240 Page 84 Operating Instructions UltiMate 3000 Series Photodiode Array Detector The following components are available as replacement parts Description PEEK P N Stainless Steel P N Reducing union fittings analytical and 6080 2101 6080 2102 semi micro cells Union fittings semipreparative cell 6080 2103 Cell outlet tubing analytical and semi 6080 2401 6080 2403 micro cells 0 38 mm 0 015 in ID 0 25 mm 0 010 in ID Cell inlet or outlet tubing 6080 2406 semipreparative cell 0 51 mm 0 020 in ID Outlet fluidic
54. cal HPLC applications Dionex recommends stacking the individual modules for example as shown in Fig 11 page 25 and interconnecting them on the rear panel However the arrangement of the system modules depends on the application NOTE Apart from the solvent rack all modules of the UltiMate 3000 system can be connected separately to the server PC However Dionex recommends interconnecting all modules and then connecting the system to the Chromeleon server PC via only one connection To do so use the USB hub on the pump or detector Page 24 Operating Instructions UltiMate 3000 Series Photodiode Array Detector WT EDIONEX EDIONEX 10 wo 5 TTT FADIONEX c A D TTT EIDIONEX Server PC Mains Line Fig 11 Example for the rear panel connections on an UltiMate 3000 system Operating Instructions Page 25 UltiMate 3000 Series Photodiode Array Detector 3 4 Installing Chromeleon Software NOTE Dionex strongly recommends installing Chromeleon before connecting the PDA 3000 to the computer When you install the Chromeleon software first the USB driver for the detector is automatically loaded and the Windows operating system can detect the detector when the power is turned on Before going on to 3 5 verify that Chromeleon is installed on the computer and a license is installed 3 5 Connecting the Detector 3 5 1 USB Connection The PDA 3000 can be connected directly to a U
55. ce e Installez le syst me HPLC dans un laboratoire bien ventil Si la phase mobile contient des solvants volatils ou inflammables emp chez qu ils ne p n trent dans l espace de travail Afin d viter au maximum les interf rences tous les l ments du syst me analytique doivent tre raccord s la m me ligne secteur m me phase e Lorsque vous soulevez ou l instrument tenez le toujours par le dessous ou par les c t s de l unit Soulever l instrument par la partie avant inf rieure ou par le panneau avant peut endommager la porte Ne placez aucun objet lourd sur la porte ouverte du panneau avant Ceci pourrait endommager la porte e Apr s utilisation purgez le syst me des tampons et des susceptibles de former des peroxydes e Sila phase mobile contient des solvants volatils ou inflammables vitez les flammes nues et les sources d tincelles proximit e Siune fuite se produit arr tez imm diatement l instrument et rem diez au probl me e Quand les capots sont d mont s des connexions lectriques sous haute tension deviennent accessibles D branchez l instrument de toute source d alimentation lectrique avant de retirer les capots e Remplacez toujours les fusibles grill s par des fusibles de rechange d origine Dionex chapitre 0 page 95 e Remplacez les cordons d alimentation lectrique et les c bles de communication d fectueux e De nombreux solvants organiques e
56. ce If the baseline noise is synchronized with the pump stroke reprime the pump and clean the piston seals and or check valves Refer to the pump user s manual for instructions e Negative absorbance level is too high Baseline noise may increase as the negative absorbance increases If the noise is unacceptable reduce the negative absorbance level page 53 5 6 Drifting Baseline e Fluctuations in ambient temperature Make sure the PDA 3000 installation site temperature remains consistent Allow at least 6 cm 2 4 in of clearance behind the PDA 3000 for ventilation Check that the flow cell inlet tubing is routed through the heat exchanger Fig 6 page 16 and is correctly connected to the inside front panel Fig 31 page 89 Check that solvent flow is directed to the cell inlet and out the cell outlet Select the active reference mode by entering a reference wavelength page 49 e Front panel lamp cover or flow cell cover is missing Optical components are sensitive to temperature and light Do not operate the PDA 3000 unless the front panel lamp cover and flow cell cover are in place e 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 Fig 30 page 88 e Lamp not stabilized or burned in The lamps usually require 20 to 30 minutes to stabilize For sensitive applications
57. ch the Found New Hardware Wizard 3 6 2 Installing the Detector After the USB software for the detector has been installed gt page 29 install and configure the detector in Chromeleon l 2 Start the Chromeleon Server Monitor if it is not already running gt page 29 Start the Chromeleon Server Configuration program by clicking Start on the taskbar Point to Programs or All Programs depending on the operating system point to Chromeleon and then click Server Configuration If necessary click the plus sign beside the server name to display the items underneath Select the timebase to which the autosampler will be assigned or create a new timebase on the Edit menu click Add Timebase Open the Add device to timebase dialog box To do so click Add Device on the Edit menu or right click the timebase and click Add Device on the menu On the Manufacturers list click Dionex HPLC UltiMate 3000 and on the Devices list click PDA 3000 Detector Chromeleon connects to the detector and transfers the settings from the instrument firmware to Chromeleon setting the options installation tab pages accordingly Page 30 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 10 On each tab page verify that the settings are correct and select additional settings if needed For a description of the tab pages click the Help button Click Finish to complete the installation of the autosampler
58. 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 Operating Instructions Page 47 UltiMate 3000 Series Photodiode Array Detector 4 3 5 Bandwidth The bandwidth defines a wavelength range around the wavelength at which the chromatogram is measured Select a bandwidth that provides the resolution required to achieve the desired sensitivity Increasing the bandwidth increases the number of different wavelength signals averaged at each point in time As the bandwidth increases baseline noise decreases however this may decrease the signal especially of those peaks that exhibit spectral peak maxima For narrow spectral peaks select narrow bandwidths Example Chromatogram Selecting the Bandwidth Fig 26 page 48 illustrates how selecting a wide bandwidth for both the sample and reference wavelengths reduces noise by averaging over a wavelength range The operating conditions are Sample wavelength 254 nm Reference wavelength Off Flowing water at 1 0 mL min 10 35 MPa 1500 psi 0 0400 fa WCET M N h on N WI nm VJ An NAUN M AA mM ANT Ah P WT WU hu W VW ha My al W wih AN NL Lan f Myla _ m Bandwidth 8 V W Noise 14 LAU i 0 01004 M h Hm o0000 Je My N
59. d post run analyses may require more processing time e A slow data collection ratewith a fast rise time may result in a longer system response than indicated by the rise time For example a data collection rate of 0 5 Hz and a rise time of 0 5 second results in a system response longer than 2 0 seconds e Ata data collection rate of 20 Hz the 3D sample wavelength range must be lt 310 nm Regardless of the data collection rate the reference wavelength if set must always be within the 3D range e The table below lists the recommended pairings for the rise time and data collection rate Rise Time Data Collection Rate seconds Hz 0 05 20 0 0 1 20 0 0 2 10 0 0 5 5 0 1 0 2 0 2 0 1 0 5 0 0 5 4 3 4 Sample Wavelength The PDA 3000 measures absorbance over all wavelengths from 190 to 800 nm The deuterium lamp optimizes the UV range 190 to 380 nm while the tungsten lamp optimizes the visible range 380 to 800 nm Set the sample wavelength at the wavelength with the absorbance maxima for the analytes of interest When the analyte wavelength maxima are known the PDA 3000 can run five separate wavelengths without being required to collect spectra Collecting individual wavelengths instead of the spectra offers two advantages it uses less disk space and it eliminates the need to perform extractions for analyses that do not require spectral data If little is known about the analytes in the sample
60. ds tesa eked ed 20 2 7 Mobile Phases ser Tdr brast ent sk renee ER en ennemie 21 2 8 Solvent Delivery System 0 cccccsseeesceesecesceeeneeeseessceeeneceaeeeseeeseeeeaeeeseenseeeeneens 21 3 Wins tallation sivsicsececesccssccscssccnvscnsetecesonscenssceaevnesenssansegnbasoscsessssusguadcenscacevavacesscostsenseasads 23 3 1 Facilities Required ics ten en east eee ede Rate etic 23 3 2 Unpacking the PDA 3000 E N a 23 3 3 Positioning the Detector in the UltiMate 3000 System cc eeeeeeeeeteeeteeeees 24 3 4 Installing Chromeleon Software cccccccccccssscesscccesseeeesesecseeceseeeseseseeseseeseeeees 26 3 5 Connecting the Detector ss 26 3 5 1 USB Connection steam inlet aa kelte Siete age Reis 26 3 5 2 Analog Output Connection ist Mantes te A ren 27 3 553 R lay T TL Connections sims aae Ee ar a E AESi 28 3 5 4 Connecting the Power Cord ss 28 3 6 Setting Up the Detector in Chromeleon ss 29 3 6 1 Loading the USB Driver for the Detector 29 3 6 2 Installing the Detector ss 30 3 7 Installing the Flow Cell 31 3 8 Connecting the Waste Tubing 33 4 D t ctor Control sissies rires sios r e een etes ete nettes ins e nee 35 4 1 Getting Started naan none tn ee Mn n
61. e 3000 Series Photodiode Array Detector 2 5 Rear Panel Fig 9 illustrates the rear panel of the PDA 3000 F Fig 9 PDA 3000 Rear Panel No Description 1 Fuse holder The fuse holder holds the two main power fuses section 6 4 page 97 2 Power receptacle for connecting the power cord section 3 5 4 page 28 3 Analog outputs BNC connectors for connecting analog instruments section 3 5 2 page 27 4 Relay TTL connector for controlling the detector during stand alone operation section 4 5 page 58 5 USB port for connecting the detector to the Chromeleon PC section 3 5 1 page 26 Operating Instructions Page 19 UltiMate 3000 Series Photodiode Array Detector 2 6 Leak Sensor Liquid leaks in the detector will be detected by the leak sensor that is installed on the inside front panel Fig 10 Leak sensor If the leak sensor detects a leak the Run LED on the front panel door is red and an error message appears on the front panel display Eliminate the leak and dry the leak sensor as described in section 6 1 gt page 83 i Tip Inspect the detector for signs of leakage every day Tighten or replace leaking connections if necessary Page 20 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 2 7 Mobile Phases Solvent quality significantly affects both detection limits and instrument perf
62. e light then passes through the slit to the grating where it is diffracted into the component wavelengths Measurement of the light occurs at the photodiode array Each diode measures a narrow portion of the spectrum Visible Focus Lens Tungsten Lamp Deuterium Lamp Flow Cell Filter Paddle Photodiode Array S Source Lens I LP HT 7 Spectrograph Lens Grating Fig 5 PDA 3000 Optical System Optical System Component Function Tungsten Lamp The light source for visible and near infrared wavelengths 380 to 800 nm The tungsten lamp is focused through an opening in the internal structure of the deuterium lamp this allows the lamps to share the optical axis to the source lens Visible Focus Lens Focuses the visible light from the tungsten lamp to the through hole of the deuterium lamp Deuterium Lamp The light source for UV wavelengths 190 to 380 nm Source Lens Receives the light from the tungsten and deuterium lamps and focuses it so that the beam passes through the flow cell Flow Cell The measurement site for sample absorbance The cell has a flat window on each side Dionex offers five cells for use with the PDA 3000 analytical cells in PEEK and 316 stainless steel semi micro cells in PEEK and 316 stainless steel and semipreparative cells in PEEK only Page 14 Operating Instructions UltiMate 3000 Series Photodiode Array Detector Optical System Component
63. e the Audit Trail from a timebase by selecting the Audit Trail folder in the timebase and the file for that date in the Chromeleon browser Chromeleon includes several diagnostic functions for monitoring the wellness of your chromatography system These functions help to prevent problems and ensure reliable operation of each module in the system e Lamp age Purpose Indicates the total number of hours that each lamp has been turned on in its lifetime To check the number of hours the lamps have been in service 1 In Chromeleon press F8 to display the Commands dialog box and select UV 2 Select UVLampAge If the deuterium lamp has been in service for more than 2000 hours replace it section 6 3 2 page 92 3 Select VisLampAge If the tungsten lamp has been in service for more than 2000 hours replace it section 6 3 3 page 95 To reset the lamp age 1 After installing a new lamp press F8 to display the Commands dialog box 2 Select UV 3 Select the UVLampAge command for the deuterium lamp or VisLampAge command for the tungsten lamp 4 Reset the number to zero 5 Click Execute NOTE When the detector power is initially turned on the lamp age already indicates some elapsed time this is the time that was required for factory calibration and test procedures e Lamp intensity Purpose Chromeleon provides counters for the UV lamp s intensity at 254 nm in counts per second and for the visible lamp s intensi
64. ecently installed a new deuterium lamp check that the UV lamp connector wires are routed through the wire guide in the optical bench Fig 35 page 93 and are not pinched under the lamp cover 3 Check the number of hours the lamp has been in service page 55 If the deuterium lamp has been in operation for more than 2000 hours replace it gt section 6 3 page 91 If the error message appears again contact Dionex Service for assistance If the deuterium lamp has been in operation for ess than 2000 hours turn off the lamp for at least 3 minutes and then turn it on again If the error message reappears replace the lamp section 6 3 page 91 If the error message does not appear again run a manual data acquisition for about 30 minutes If you notice a shift in the absorbance signal during this time replace the lamp If the tungsten lamp has been in operation for more than 2000 hours replace it gt section 1 page 92 If the error message appears again contact Dionex Service for assistance If the tungsten lamp has been in operation for ess than 2000 hours turn off the lamp for at least 30 seconds and then turn it on again If the error message reappears replace the lamp gt section 1 page 92 If the error message does not appear again run a manual data acquisition for about 30 minutes If you notice a shift in the absorbance signal during this time replace the lamp UV lamp control circuitry error while la
65. ed 4 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 5 Remove the two crosshead screws that hold the metal connector cover on the right in place and then remove the cover and set it aside Page 92 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 6 10 11 Squeeze the clip on the UV lamp connector Fig 35 and disconnect it from the 6 pin bulkhead connector on the side wall Locating pins UV lamp connector Vis lamp connector Fig 35 Lamp Connections Loosen the three screws in the deuterium lamp flange and pull the lamp out of the optical bench NOTE _ The screws are captive in the lamp base and do not need to be removed Inspect the new deuterium lamp for fingerprints and dust If necessary clean the lamp with isopropyl alcohol Line up the flange of the new lamp with the two locating pins and three threaded holes in the optical bench Fig 35 When the flange is aligned gently push the lamp into the optical bench NOTE As opposed to many other optical detectors the PDA 3000 deuterium lamp forward light beam points away from the flow cell when installed correctly 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 Squeeze the clip on the UV lam
66. el di loirainar iinnt 21 Rear Panel Connections 28 Recorder entame 29 81 Reference Bandwidth 44 46 Definition aenar auda anua 52 Guidelines for Selecting 50 51 52 Reference Intensity u dssceueeeeeerersenrensnene 51 Reference Modes ccccccssecseesseesssesseeseeeseeeees 51 Active Reference Mode cccccccesseseeeees 51 Active Reference Wavelength 76 Reference Wavelength sss0 0se0s 44 46 51 52 Definitions senser ninina a 51 Guidelines for Selecting 51 Inappropriate Setting 75 Relay and TTL Connector sscecrerrreree 105 Relay Control 30 105 Rise ME reines wel aeara 44 46 Correlation with Data Collection Rate 49 Definitions sis sakrale ASE 47 Effect on Baseline Noise 47 Guidelines for Selecting 47 49 Inappropriate Setting 75 RMA Numbers nent 85 Run LED 13 71 Safety Icons Caution fair deb eine Sample Bandwidth 0 eee eee 50 Sample Intensity 31 Sample Rate see Data Collection Rate 48 Sample Wavelength Sample Wavelength Semi Micro Flow Cell Semipreparative Flow Cell Sensitivity Separator Column Service Procedures Cell Cleaning 2 3 rss 8
67. ength calibration to fail Operating Instructions Page 77 UltiMate 3000 Series Photodiode Array Detector 5 9 Wavelength Verification Fails e Detector wavelength requires recalibration Open the PDA 3000 Wellness panel and run the wavelength calibration procedure page 56 e No solvent flow through cell If the Power LED is flashing Fig 3 page 11 flush the cell with DI water or methanol and then turn off the detector power for 30 seconds Turn on the power again and verify that the Power LED is no longer flashing Check the Audit Trail If the Not enough light to perform operation message is displayed flush the cell with DI water or methanol until the autozero routine can be performed without error e Lamp s needs replacement Check the number of hours the lamps have been in service gt page 55 and replace them if necessary e Solvent absorbs at the wavelength reported for verification Pump DI water or methanol through the system during the wavelength verification test e Filter paddle position error Check the Audit Trail If the Filter wheel sensor could not detect blocked position or Filter wheel sensor could not detect open position message is displayed see page 65 for instructions 5 10 No Spectra Collected e Spectral range was not programmed In Chromeleon select a spectral range in the PGM file or on the PDA 3000 Control panel Page 78 Operating Instructions UltiMate
68. eon press F8 to display the Commands dialog box b Select UV and UV _Calibration c Select Intensity and click Execute to calibrate the lamp intensity d Select Autozero in the Commands dialog box and click Execute to run the autozero routine e If no error message is displayed flush the cell with the mobile phase for the application and or clean the cell as instructed in Section 6 2 page 84 f Reinstall the cell in the optical bench g Autozero the detector again to verify that the problem has been resolved If the error message appears again contact Dionex Service for assistance If the intensity reading is below 10 million counts for an analytical or semipreparative cell or below 3 million counts for a semi micro cell follow these steps a Check that the flange of the deuterium lamp is aligned with the two locating pins in the optical bench gt Fig 35 page 93 If the flange is aligned the lamp is defective and should be replaced section 6 3 page 91 b If the error message appears again contact Dionex Service for assistance e Flow cell contains air bubble or old mobile phase Flush the cell with the mobile phase for the application e Cell not clear Clean the cell section 6 2 page 84 If the detector fails the wavelength calibration again replace the flow cell windows section 6 2 5 page 89 Contaminated flow cell windows can significantly increase baseline noise and cause wavel
69. erating Instructions Page 59 UltiMate 3000 Series Photodiode Array Detector 5 1 Alarms and Error Conditions The PDA 3000 Firmware periodically checks the status of certain system parameters If a problem is detected it is reported to the Chromeleon PC and displayed in the Chromeleon Audit Trail Each error message is preceded by an icon that identifies the seriousness of the underlying problem see the table below You can change the severity level assigned to a problem whenever appropriate Description A message is displayed in the Audit Trail but the current run is not interrupted A message is displayed in the Audit Trail and the system attempts to correct the problem sometimes by using an alternative parameter A message is displayed in the Audit Trail and the running batch is aborted The table below lists the PDA 3000 error messages and their default severity levels For troubleshooting assistance refer to the page indicated in the table Alarms and Error Conditions Default Severity Level See 3DFIELD RefWavelength and or RefBandwidth is out of Error page 62 range Acquisition On for 3DFIELD rejected no 3D Data Abort page 63 Acquisition icense found Autozero is already in progress page 63 Calibration is running page 63 Cannot change 3DFIELD parameters while data acquisition Warning page 63 is running Cannot set manual parameters for the required operation Abort pa
70. ese operating instructions For the general safety precautions in French refer to Consignes G n rales de S curit gt page 5 To avoid the possibility of personal injury and or damage to the instrument observe the following general safety precautions when operating the detector or carrying out any maintenance work Please observe the following general safety precautions when operating the instrument or carrying out any maintenance work e Install the HPLC system in a well ventilated laboratory If the mobile phase includes volatile or flammable solvents do not allow them to enter the workspace e For minimum interference effects all components of the analytical system should be connected to the same mains output same phase e The front panel door tilts downward To prevent damage to the detector when lifting or moving always lift only from the bottom or by the sides The open front panel door is not designed to carry weight Therefore you should not place any objects on the open door e After operation rinse out buffers and solutions that form peroxides Operating Instructions Page 3 UltiMate 3000 Series Photodiode Array Detector e Ifthe mobile phase includes volatile or flammable solvents avoid open flames and sparks e Ifa leak occurs turn off the instrument and remedy the situation immediately e When the panels are removed dangerous electrical connections will be exposed Disconnect the detector fr
71. esponse time is approximately the larger of a the rise time or b two times the step size when average is On Operating Instructions Page 53 UltiMate 3000 Series Photodiode Array Detector 4 3 11 Negative Absorbance Negative absorbance is the result of decreased baseline absorption of the mobile phase after the autozero routine which usually occurs at the beginning of a run At the default setting of 1 the PDA 3000 becomes saturated when the light transmission is 20 above the autozero level This results in a flat truncated baseline If desired increase the negative absorbance level in order to continue seeing the actual baseline and peaks This is especially helpful when running a gradient application in which the absorbance decreases more than 100 mAU As the following table indicates the extent of negative absorbance depends on the wavelength The values in this table are intended as guidelines only Negative Approximate Approximate Approximate Absorbance Level Negative Absorbance Negative Absorbance Negative Absorbance at 210 nm at 240 nm at 254 nm 0 2200 mAU 50 mAU 300 mAU 1 default 2300 mAU 100 mAU 350 mAU 2 2600 mAU 200 mAU 450 mAU 3 2600 mAU 300 mAU 550 mAU 4 2700 mAU 400 mAU 630 mAU 5 2700 mAU 500 mAU 660 mAU 6 2700 mAU 600 mAU 760 mAU These signals are saturated and will not report a further negative value 1 In Chromeleon press F8 to display the Com
72. g Instructions UltiMate 3000 Series Photodiode Array Detector PDA 3000 Command Step TTL Input Mode UV Lamp UVLampAge UVLampPowerOnSetting Visible_Lamp VisLampAge VisLampPowerOnSetting Wavelength WavelengthCal WavelengthCalResult WavelengthVerTest WavelengthVerTestResult Function Sets the step which is the time interval between two successively stored data points in the chromatogram page 52 Sets the TTL input signal mode Turns the deuterium lamp on and off Reports or resets the number of hours the deuterium lamp has been on Selects the power up setting for the deuterium lamp i e whether the lamp is turned on whenever the detector is turned on The default setting is On Turns the tungsten lamp on and off Reports or resets the number of hours the tungsten lamp has been on Selects the power up setting for the tungsten lamp i e whether the lamp is turned on whenever the detector is turned on The default setting is On Sets the sample wavelength up to five sample wavelengths can be programmed page 47 Runs the wavelength calibration procedure to improve wavelength accuracy in the UV range The result of the last wavelength calibration procedure Performs the wavelength verification test via the holmium oxide filter The result of the last wavelength verification test Operating Instructions Page 43 UltiMate 3000
73. ge 64 because the DSP is not ready Can t execute calibration command during data acquisition page 64 Can t execute diagnostic command during data acquisition page 64 Can t execute X command during data acquisition page 64 Command not executed because an Autozero command is Warning page 64 already running Data is unavailable page 64 Diagnostic is running page 64 DSP communication failure Abort page 65 Page 60 Operating Instructions UltiMate 3000 Series Photodiode Array Detector Alarms and Error Conditions Default Severity Level See Filter wheel sensor could not detect blocked position Warning page 65 Filter wheel sensor could not detect open position Warning page 65 Invalid rise time Valid rise times at 20Hz 0 05 0 1 0 2 Abort page 65 0 5 1 0 and 2 0 Invalid step for the 3DFIELD Valid steps are 0 05 0 1 0 2 Error page 66 0 4 0 5 1 2 and 4 Leak sensor error Warning page 66 Not enough light to perform operation Warning page 66 Over temperature error Abort page 66 PDA is running a calibration or diagnostic function Not Error page 67 ready to accept this command The minimum wavelength must be less than the maximum Error page 67 wavelength Min wavelength X max wavelength X The range of wavelength bunching is 1 to 25 nm Error page 67 The range of wavelengths is outside the 190 to 800 nm limit Error page 67 Wavelength X Bandwidth X UV lamp control c
74. ge appears if you select Autozero in the Commands dialog box when the autozero routine is already in progress Allow the autozero routine to continue running until completion Calibration is running To troubleshoot This message appears if you attempt to issue a command or select a parameter while a calibration procedure is in progress Wait until the procedure finishes running before making any changes Cannot change 3DFIELD parameters while data acquisition is running To troubleshoot This message appears if you attempt to select a parameter for the 3D field while data acquisition is in progress Wait until data acquisition is complete or stop the run and then change the parameters Operating Instructions Page 63 UltiMate 3000 Series Photodiode Array Detector Cannot set manual parameters for the required operation because the DSP is not ready To troubleshoot This message appears if certain commands are issued before the DSP digital signal processor is ready to accept them Turn off the PDA 3000 power for 30 seconds and then turn it on again If the error message appears again contact Dionex Service for assistance D Can t execute calibration command during data acquisition A Can t execute diagnostic command during data acquisition Can t execute X command during data acquisition To troubleshoot During data acquisition no other commands can be executed Wait until data acquisition is
75. idth 44 46 54 C Cable USB a hae 28 Calibration wavelength scenerne 58 Cells lasere nie 16 17 46 47 Air Bubble Prevention 74 Air Bubble Removal 88 Backpressure Line 74 Chemical Compatibility 17 46 47 Cleaning ARS SER ein nn nie 88 Heat Exchangers ooseson ninien 18 19 Installation sense 33 Leakage Check 0 ecceeseeseeceeseeereeeeeeeneeees 93 Replacement Service Procedures 86 Wid w Sann nn eee 16 Windows and Seals Replacement 91 Chlorinated Solvents cccccccessccesseceesseeeenees 17 Chromeleon Audit Trail Commands ssscerererererererrerenerer nerne Commands Dialog Box Contr les Detector Installation Diagnostics Installation Program Lamp Diagnostics uu u sssscerererserrerrernnee Load USB Driver PDA Control Server Configuration Program Server Monitor 31 Commands Dialog Box ssec 44 Connection ANALOG a b coacsstsiesdeskeebesneasdiatoun est ateseok ence Power Cordes Relay TTL Connection USB idee te sn date Connections Control Commands Co trol Panels Ae D Dark Signal 17 Data Collection Rate 44 46 Definition Guidelines for Selecting sc 48 49 Relationship to Step 54 Data Points Deuterium Lamp AGE sirhrsares Calibration F
76. ine finishes running before attempting to issue any command A The minimum wavelength must be less than the maximum wavelength Min wavelength X max wavelength X To troubleshoot Select a minimum wavelength that is less than the maximum wavelength Both wavelengths must be within the 190 to 800 nm range A The range of wavelength bunching is 1 to 25 nm To troubleshoot This message appears if you enter an invalid setting for the bunch width Select a bunch width setting from 1 to 25 nm The range of wavelengths is outside the 190 to 800 nm limit To troubleshoot The PDA 3000 can measure the absorbance spectrum from 190 to 800 nm Make sure both the minimum and maximum wavelengths are within this range UV lamp error UV lamp error or control circuitry error while lamp is on UV lamp failed to turn on for the required operation UV lamp error while attempting to turn on Visible lamp error Visible lamp error or control circuitry error while lamp is on Visible lamp error while attempting to turn on Visible lamp failed to turn on for the required operation Operating Instructions Page 67 UltiMate 3000 Series Photodiode Array Detector To troubleshoot 1 Check that the lamp referred to in the error message is turned on When a lamp is on the corresponding front panel LED Deuterium or Tungsten is lighted If necessary turn on the lamp from either Chromeleon or the TTL input 2 If you r
77. ing 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 A Avertissement DANGER D ELECTROCUTION ET D INCENDIE Le module d alimentation lectrique fonctionne aux potentiels du secteur Faites effectuer toutes les r parations par un personnel qualifi 3 5 4 Connecting the Power Cord The PDA 3000 power entry is socketed for a modular power cord IEC 320 C13 The detector operates from input voltages over a range of 85 to 265 VAC 47 to 63 Hz power and requires a grounded single phase power source The typical input power is 100 W and the maximum line draw is 3 5 amps at 110 VAC when the detector power is turned on The appropriate line voltage and frequency are selected automatically A Warning SHOCK HAZARD To avoid electrical shock use a grounded receptacle Do not operate the PDA 3000 or connect it to AC power mains without an earthed ground connection VAN Caution The power supply cord is used as the main disconnect device Make sure the socket outlet is located near the PDA 3000 and is easily accessible Page 28 Operating Instructions UltiMate 3000 Series Photodiode Array Detector VAN Avertissement DANGER D LECTROCUTION 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
78. ion of the base is greater than 50 mM disconnect the separator column and flush the system with DI deionized water for 5 minutes at 1 0 mL min immediately after the analysis If strong base remains in the cell for 1 or 2 days the cell windows may need to be replaced section 6 2 5 page 89 Do not use a PEEK flow cell with normal phase or chlorinated solvents these solvents will damage the cell Do not use the stainless steel flow cell with low pH solutions these solutions may cause corrosion contamination and metal leaching 4 3 2 Rise Time Rise time is a measure of how quickly the PDA 3000 responds to a change in signal The rise time settings are 0 05 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 is 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 Fig 25 page 46 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 Operating Instructions Page 45 UltiMate 3000 Series Photodiode Array Detector Rise Time 0 5 sec Baseline Noise 22 AU 00250 ImAU WVL 254 nm 0 0100 0 00
79. ions Page 39 UltiMate 3000 Series Photodiode Array Detector 10 11 12 13 14 To program 3DFIELD the 3D channel a Check or clear a check box to determine whether 3D data will be collected b Ifthe channel is selected enter the starting and ending data acquisition times as well as the reference wavelength and reference bandwidth NOTE The reference wavelength if set must be within the 3D range The total of the reference wavelength plus one half the reference bandwidth must always be within the sample wavelength range selected if it is not the reference wavelength will default to the longest wavelength Enter the 3D Min Wavelength and 3D Max Wavelength NOTE If the data collection rate is 20 Hz the 3D sample wavelength range must be lt 310 nm Enter the 3D Bunchwidth the distance between wavelengths Click Next to continue The following screen is displayed The tree control lists states for all devices in the selected timebase Click the plus sign to the left of a device name to expand or collapse the struture and view the device states Program Wizard Relay and State Devices Options x E UV Relay 1 Retention Time min Add Q Open State Open 7 Delete 94 Closed BU Rely 2 Time Deve ome Dustin E UV TTL 1 a e UV TTL 2 Help nates or sets the device s state lt Back Cancel Help Fig 23 Program Wizard Relay and State Device Options NOTE
80. ircuitry error while lamp is off Abort page 68 UV lamp error or control circuitry error while lamp is on Abort page 67 UV lamp error Abort page 67 UV lamp error while attempting to turn off Abort page 68 UV lamp error while attempting to turn on Abort page 67 UV lamp failed to turn on for the required operation Abort page 67 Visible lamp control circuitry error while lamp is off Abort page 68 Visible lamp error or control circuitry error while lamp is Abort page 67 on Visible lamp error Abort page 67 Visible lamp error while attempting to turn off Abort page 68 Visible lamp error while attempting to turn on Abort page 67 When collecting at 20Hz the spectrum range cannot be Abort page 69 more than 310 nm Please lower the data rateor narrow the spectrum range Operating Instructions Page 61 UltiMate 3000 Series Photodiode Array Detector A 3DFIELD RefWavelength and or RefBandwidth is out of range To troubleshoot For all data collection rates other than 20 Hz select parameters that meet the following criteria 1904 At 300 Where Reference wavelength BW Reference bandwidth For example the following parameters are VALID Wavelength 190 to 800 nm Reference wavelength 750 nm Reference bandwidth 50 nm These parameters are valid because 750 nm 25 nm 50 of 50 nm 775 nm which is less than 800 nm The following par
81. is lighted Page 70 Operating Instructions UltiMate 3000 Series Photodiode Array Detector Lamp LED flashing The corresponding lamp failed to power on properly In Chromeleon press F8 to display the Commands dialog box and select UV Check that the command UVLampPowerOnSetting or VisLampPowerOnSetting is On If the LED continues flashing replace the lamp See section 6 3 page 91 or section 1 page 92 for instructions on replacing the deuterium lamp or tungsten lamp respectively Detector and or Control panel not connected to timebase In the Chromeleon Server Configuration program add the PDA 3000 driver to a timebase For details refer to the section on the Server Configuration Program in the Chromeleon Administrator Help Windows operating system does not recognize PDA 3000 When the computer is turned on Windows scans the network for unknown devices If the PDA 3000 power is off the detector cannot be identified If you connect the PDA 3000 to the computer before installing Chromeleon a Windows message box requesting a USB configuration file cmwdmusb inf will appear when you turn on the computer See Section 5 14 page 81 for instructions on how to resolve this 5 5 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 DI water
82. k the Audit Trail If the Filter wheel sensor could not detect blocked position or Filter wheel sensor could not detect open position message is displayed see page 65 for instructions e Failure of an electronics component Turn off the PDA 3000 power and contact Dionex Service for assistance NOTE Do not attempt to service the PDA 3000 electronics components All repairs of the electronics components must be performed by a Dionex Service Representative 5 8 Wavelength Calibration Fails e Deuterium lamp may be defective If the Deuterium LED is flashing or if the LED fails to light replace the deuterium lamp section 6 2 4 page 87 If the Deuterium LED is lighted but is not flashing open the PDA 3000 Wellness panel and run the wavelength calibration and the wavelength verification test If the PDA 3000 fails these procedures remove the flow cell from the detector and repeat both procedures If the detector fails the wavelength calibration again contact Dionex Service for assistance Page 76 Operating Instructions UltiMate 3000 Series Photodiode Array Detector e Deuterium lamp intensity out of calibration 1 Remove the cell from the optical bench section 6 2 4 page 87 2 Check the deuterium lamp intensity page 55 If the intensity reading is above 10 million counts for an analytical or semipreparative cell or above 3 million counts for a semi micro cell follow these steps a In Chromel
83. kpressure 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 DI water immediately after the analysis 2 8 Solvent Delivery System The pumping system should deliver continuous flow while maintaining a consistent mobile phase composition if gradient elution is used Fluctuations in system backpressure may cause baseline disruptions High sensitivity applications require a smooth low pulsation pump To ensure optimal results follow the maintenance schedule recommended in the pump user s manual All materials in the solvent delivery system must be fully compatible with the mobile phases required for the analysis For example IC and BioLC analyses frequently use mobile phases with extreme pH levels or high salt concentrations A PEEK pumping system and PEEK flow cell are required when running these mobile phases because the presence of stainless steel in the flow path would contaminate the system Operating Instructions Page 21 UltiMate 3000 Series Photodiode Array Detector Reversed phase solvents methanol moderate concentrations of acetonitrile etc are acceptable for a PEEK system Other solvents and high concentrations of acetonitrile require a stainless steel system All tubing connections should be Teflor Tefzel PEEK stainless steel or titanium as required for the specific operating pressures and
84. lacing the Analytical or Semi Micro Flow Cell Light inlet side shown 4 Remove and discard the old window Operating Instructions Page 89 UltiMate 3000 Series Photodiode Array Detector 10 11 Use a needle to carefully remove the seal from the groove Do not scratch the groove or cell body Scratches will prevent the new O ring from sealing properly and cause leakage Fig 32 Removing the seal from the groove The following factors will prevent the new O ring from sealing properly and will cause leaks scratches in the groove particles of dust or dirt in the groove and failure to seat the new O ring in the groove Check the groove to be sure it does not contain any dust or dirt particles and then carefully press the new seal into the groove Do not use a sharp tool as this may damage the seal Make sure the seal is seated correctly in the groove Place a new window into the counterbore in the retaining nut Screw the nut and window into place from below as shown in Fig 33 Fig 33 Placing a new window Using the windows replacement tool tighten the retaining nut until snug and then turn an additional one quarter turn Repeat Step 3 through Step 8 to install the second window Check the flow cell for leakage gt page 91 Reinstall the flow cell in the optical bench page 29 Page 90 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 6 2 6 Checking the Flow Cell
85. length verification fails eeeee 80 UV Wavelengths rocoh 16 TET Control cr none 30 105 TTL Input Mode cl coke ces 45 V Tubing Connections ise ask ns 2A 85 86 87 Ventilation ste ins a i 76 Tungsten Lampione neies 10 16 i i Dee Pint Pes chad tigi ceesi SENE ES 45 YEr A Aan WAV Elen susan goatee eee Visible Focus Lens 16 Calibration sserrsemssssurtemenmnmsnennues 78 Visible Waveleneths 16 Failures eder mure duree 14 rt nr Tntensity renare 57 W Lamp does not light 1 72 On Off Control 45 Warranty Voiding 85 Output Waning 74 Waste Tubing iis skeder Retenir 35 Replacing semer 97 Wavelength ssssausnssunne 10 45 Time to Stabilize c eee 37 73 76 Wavelength Calibration 45 58 80 Tungsten LED 71 72 73 Wavelength Verification 17 45 59 Wavelengths single 49 51 U Unpacking Instructions 25 Page 108 Operating Instructions
86. lso be operated with other data systems such as Analyst Applied Biosystems MDS Sciex HyStar Bruker Daltonics or Xcalibur Thermo Scientific To do so installation of the DCMS Dionex Chromatography Mass Spectrometry Link software is required To take full advantage of the capabilities of the PDA 3000 order Chromeleon with the PDA Control option This option is required in order to perform e 3D data presentation and spectral analysis real time or post run e Peak purity analysis with selectable criteria e Spectral library search for positive peak identification Operating Instructions Page 7 UltiMate 3000 Series Photodiode Array Detector 1 4 Theory of Photodiode Array Detection Monochromatic variable wavelength detectors monitor eluting components of the sample at a single wavelength ideally the wavelength of maximum absorbance Photodiode array PDA detectors scan a range of wavelengths every few milliseconds and continually generate spectral information Wavelength time and absorbance can all be plotted For example Fig 1 page 8 shows an overlay of pyrene and an impurity obtained from two consecutive chromatographic analyses Based on 2D data or if the analyses had been performed with a conventional variable wavelength detector these peaks might have been misidentified as the same component A PDA 3000 under the control of Chromeleon with the PDA Control option correctly identified and differe
87. mands dialog box 2 Select UV and then select NegativeAbsorptionLevel Enter a new setting and click Execute 3 Select Autozero in the Commands dialog box and click Execute to run the autozero routine 4 Select LampIntensity in the Commands dialog box to check the intensity of the deuterium lamp The reading should be above 10 million counts for an analytical or semipreparative cell or above 3 million for a semi micro cell If the reading is below 10 million counts select UV_Calibration Intensity and click Execute to calibrate the intensity of the deuterium lamp Afterward check the lamp intensity again If the reading is still too low clean the flow cell section 6 2 page 84 or replace the lamp section 6 3 page 91 5 You may continue increasing the negative absorbance level if the range is required however be aware that baseline noise may increase as the negative absorbance increases Page 54 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 4 4 Wellness and Diagnostics The PDA 3000 Firmware periodically checks the status of certain system parameters All problems are reported to the computer and logged in the Chromeleon Audit Trail The Audit Trail includes the date time and severity level for each problem the PDA 3000 reports There are two ways to review this information e Check the Audit Trail displayed in the PDA 3000 Control panel or e Retriev
88. mp is off UV lamp error while attempting to turn off Visible lamp control circuitry error while lamp is off Visible lamp error while attempting to turn off To troubleshoot The lamp power supply may have failed or the CPU board may have failed Contact Dionex Service for assistance NOTE The PDA 3000 electronics cannot be serviced by users All repairs of the electronics components must be performed by a Dionex Service Representative Page 68 Operating Instructions UltiMate 3000 Series Photodiode Array Detector When collecting at 20 Hz the spectrum range cannot be more than 310 nm Please lower the data rate or narrow the spectrum range To troubleshoot Reduce the data collection rate to less than 20 HZ or select a wavelength range that is lt 310 nm 5 2 Flashing LED Run LED is flashing The leak sensor in the drip tray may have been triggered Check the Chromeleon Audit Trail for a leak related error message Find and eliminate the source of the leak Deuterium LED is flashing The lamp did not power on properly Check the Chromeleon Audit Trail for a lamp related error message If necessary replace the lamp section 6 3 page 91 If the LED flashes again there may be a bad connection between the lamp power supply and the lamp Contact Dionex Service for assistance NOTE The PDA 3000 electronics cannot be serviced by users All repairs of the electronics components must be perfo
89. n perform the QualificationDone command to update the Qualification LastDate and LastOperator information Operating Instructions Page 57 UltiMate 3000 Series Photodiode Array Detector 4 5 Stand Alone Analog Operation This section describes limited stand alone operation of the PDA 3000 when the detector is not interfaced to a computer running Chromeleon In stand alone operation TTL inputs on the PDA 3000 rear panel can be used to trigger autozero or to turn the lamps on and off All other detector parameters will remain at their factory default settings and cannot be changed Factory Default Settings The PDA 3000 outputs four analog signals at all times even when the detector is not interfaced to a computer Data is presented at the analog output channels whenever the detector power is on A chart recorder or other voltage measuring device can be used to monitor the channels When the PDA 3000 power is first turned on the analog output settings are at the factory defaults listed in the table below Channel Single Bandwidth Reference Full Scale Offset Wavelength Wavelength Output 1 10 2 10 3 10 4 520 10 Off 1 0 AU 10 The following default settings are also in effect when the power is first turned on e Rise time 2 0 seconds e Lamp status The deuterium and tungsten lamps are on Stand Alone Operation The table below indicates which PDA 3000 parameter e
90. ntiated the components The spectra of pyrene and the impurity clearly indicate that the two peaks are different components gt Fig 2 page 9 1 Calibration 5 Solvent Injection UV VIS 1 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 Fig 1 Overlay of Pyrene and an Impurity Page 8 Operating Instructions UltiMate 3000 Series Photodiode Array Detector Calibration 4 Compound Mix 20 0 pl Pyren 3 51 Pyren 3 52 Impurity Fm Pyrene 200 250 300 350 400 450 500 595 Fig 2 Spectra of Pyrene and an Impurity PDA detectors provide three dimensional information that allows an accurate assessment of peak identity purity and quantitation in a single analysis Software support for PDA detectors includes peak purity and spectral library search functions to help determine peak homogeneity and identity Operating Instructions Page 9 UltiMate 3000 Series Photodiode Array Detector Page 10 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 2 Description 2 1 Front Panel Fig 3 illustrates the PDA 3000 Photodiode Array Detector front panel e Press the Power switch in the lower left corner for on off control of the detector power e The four LED indicators identify the status of the detector power the deuterium and tungsten lamps and the analysis see table below When the corresponding function is in progre
91. om all power sources before removing the panels Always replace blown fuses with original spare part fuses from Dionex section 6 4 page 97 e Replace faulty power cords and communication cables e Many organic solvents and buffers are toxic Know the toxicological properties of all mobile phases that you are using e The toxicological properties of many samples may not be well known If you have any doubt about a sample treat it as if it contains a potentially harmful substance e Wear goggles when handling mobile phases or operating the instrument An eye wash facility and a sink should be close to the unit If any mobile phase splashes on the eyes or skin wash the affected area and seek medical attention e Dispose of all waste mobile phase in an environmentally safe manner that is consistent with all local regulations Do not allow flammable and or toxic solvents to accumulate Follow a regulated approved waste disposal program Never dispose of flammable and or toxic solvents through the municipal sewage system e Use only standard solvents HPLC grade and buffers that are compatible with all parts that may be exposed to solvents e In an UltiMate 3000 system some components are made of PEEK While this polymer has superb chemical resistance to most organic solvents it tends to swell when in contact with trichlormethane CHCH dimethyl sulfoxide DMSO or tetrahydrofuran THF In addition it is attacked by concentrated acid
92. om the Chromeleon menu bar toolbars and Control panels Direct control commands are executed as soon as they are entered Parameters can be modified at any time during manual data acquisition l Start the Chromeleon Server by double clicking the Server Monitor icon on the taskbar Start Chromeleon by selecting Start gt Programs gt Chromeleon gt Chromeleon The main window and the Browser will appear Select Default Panel Tabset from the View menu or click the icon on the standard toolbar The Connect to Chromeleon Server dialog box opens Select the chromatography server on which the chromatography system timebase you want to control is configured and click OK The panel tabset opens The panel tabset consists of a set of default control panels organized on tab pages If there are multiple chromatography systems connected to the selected server the window displays a panel tabset for each system Click the PDA tab to open the PDA 3000 control panel 35 Panel Tabset2 LENU3000 32 Home Sequence Control Pump Sampler Col Comp PDA Commands Signals On line Plot manual 1 Manual Acquisition F More Options Qualification Relays Inputs Ret Time Audit Trail 14 12 39 2 722 PumpLeft 96B 14 3 14 12 42 2 777 PumpLeft 96B 25 0 R14 12 43 2 799 PumpLeft 96C 10 7 1 000 pl from Pos RAL Fig 19 PDA 3000 Control Panel Example Page 36 Opera
93. ons 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 Page 22 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 3 Installation 3 1 Facilities Required Make sure the PDA 3000 installation site meets the power and environmental specifications listed in section 7 page 97 Optical detectors are sensitive to vibrations Install the PDA 3000 on a sturdy workbench in an environment that is vibration free Allow at least 6 cm 2 4 in behind and to the sides of the detector for ventilation to cool the electronics and dissipate the heat generated by the lamps Optical detectors are sensitive to changes in temperature and light Protect the PDA 3000 the columns and all tubing connections from drafts Do not operate the PDA 3000 unless the front panel lamp cover and flow cell cover are in place 3 2 Unpacking the PDA 3000 All electrical and mechanical components of the detector are carefully tested before the instrument is shipped from the factory After unpacking please inspect the instrument for any signs of mechanical damage which might have occurred during transit NOTE Immediately report any shipping damage to both the incoming carrier 1 2 and
94. ormance To ensure optimal performance of the PDA 3000 observe the following precautions 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 DI deionized water for 5 minutes at 1 0 mL min immediately after the analysis If strong base remains in the cell for 1 or 2 days the cell windows may need to be replaced section 6 2 5 page 89 Do not use a PEEK flow cell with normal phase or chlorinated solvents these solvents will damage the cell Do not use the stainless steel flow cell with low pH solutions these solutions may cause corrosion contamination and metal leaching Prepare all mobile phases with spectroscopy grade solvents reagent grade chemicals and ASTM Type I or better filtered DI 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 suppression and compound detection techniques compare the UV cutoff of the mobile phase before and after the suppressor to see whether it is advantageous to locate the PDA 3000 ahead of the suppressor This location also limits suppressor exposure to bac
95. p connector and insert it into the 6 pin bulkhead connector on the side wall Operating Instructions Page 93 UltiMate 3000 Series Photodiode Array Detector 12 13 14 15 16 17 18 Replace the lamp cover Route the wires through the guides on the lamp cover inside Fig 36 Replacing the lamp cover Do not pinch the UV lamp connector wires under the lamp cover Replace the flow cell and flow cell cover gt page 31 Close the detector front door Turn on the detector power Start the Chromeleon server Reset the lamp lifetime page 55 Run the wavelength calibration page 56 and wavelength verification test page 57 for the new lamp NOTE Allow the new lamp to run in for 24 hours minimum before the first analysis During this period strong baseline fluctuations and increased noise may occur Page 94 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 6 3 3 Replacing the Tungsten Lamp Description Tungsten lamp 6080 2002 A Caution 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 A Mise en garde 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 1 Turn off the detector power
96. pe Concentration of standard is too high column is overloaded Dilute the standard Install a smaller sample loop or inject 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 see page 47 Incorrect reference wavelength selected Select a different reference wavelength For guidelines to follow when selecting the reference wavelength see page 49 Bandwidth too wide Select a bandwidth that provides the resolution required to achieve the desired sensitivity Narrow spectra peaks require narrow bandwidths A wider bandwidth reduces baseline noise but may reduce peak height Reference bandwidth too wide Select a bandwidth that provides the resolution required to achieve the desired sensitivity A wider bandwidth reduces baseline noise but may increase the chance that the sample absorbs in the reference bandwidth thus causing reduced sensitivity and peak height Page 80 Operating Instructions UltiMate 3000 Series Photodiode Array Detector Cell flow is reversed Check that the flow cell inlet tubing is routed through the heat exchanger Fig 6
97. perating Instructions UltiMate 3000 Series Photodiode Array Detector 1 3 Product Overview The Dionex PDA 3000 Photodiode Array Detector is an optical detector capable of measuring the absorbance spectrum from 190 to 800 nm A deuterium lamp optimizes the UV range 190 to 380 nm and a tungsten lamp optimizes the visible range 380 to 800 nm When using the PDA 3000 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 e It eliminates the need to perform extractions for analyses that do not require spectral data e It conserves disk space Key features of the PDA 3000 include e The deuterium and tungsten lamps ensure low baseline noise high signal intensity and applications flexibility in the wavelength range from 190 to 800 nm e A 1024 element photodiode array optimizes spectral resolution e A built in holmium oxide filter verifies wavelength calibration accuracy e Five flow cells are available for analytical semi micro and semipreparative applications e The front panel LEDs indicate detector status at a glance e Four analog outputs support data collection on alternate data collection systems The PDA 3000 communicates with the computer through USB Universal Serial Bus It is controlled remotely by a computer running the Chromeleon Chromatography Management System However it can a
98. r a 35 4 2 Routine Operation by Chromeleon ccccceeccceeessceessseeeseeeeeeeeesseeeseeesseeeeseeees 35 RE Direct Control sa ore sate cashes daa arne dents oser rer denen renen Pee es 36 42 2 Automated Controle entit 37 42 3 Control Eommands ninss srl 42 Operating Instructions Page i UltiMate 3000 Series Photodiode Array Detector 4 3 Optimizing Detector Performance u ssssseseeeeeeererererrrr en eren ert tret errn erne 44 43 1 Flow Cell Material ae rr e a E seeren 45 43 2 Rise TIME ore es Line rire ED er aendret ete Ponte Er 45 4 3 3 Data Collection Rate visi sienne inner errant 46 4 3 4 Sample Wavelength ienna a eee ee a itede eei etaa 47 4 3 3 Bandwidth ienes AE E a 48 436 Reference Wavelengths oeisio erea a aaa ate esset OE A E A Ee 49 4 3 7 Reference Bandwidth ss his inner dn ra mal ee 50 43 8 Bono Width s et ee ne cure lata tad tn tr ec 52 430 Step sn orne a ERE ele te et en ee nt entr es eN sien a 52 4 3 10 IES Va 11 EN nest lien tentes AN lt ment ile 53 4 3 11 Negative Absorbance ss 54 4 4 Wellness and Diagnostics cccceccscesessccssseeeeseesenscesseeceseeesseeesaeeeeteeeneteeesseeenss 55 4 5 Stand Alone Analog Operation 58 5 Troubleshooting cssccsssssscssecssecsseeessscscesssscnssscscssossssssesssssesssoesesssesssesesssseseoess 59 5 1 Alarms and Error Conditions scanner reels 60 5 2 Flashing LED rasta eh in men A SE SES at vate eae 69 5 3 L
99. ration of each module in the system as well as to monitor and document service and qualification measures Section 4 4 describes some of the most frequently used diagnostic procedures Operating Instructions Page 91 UltiMate 3000 Series Photodiode Array Detector 6 3 2 Replacing the Deuterium Lamp Deuterium lamp 6080 2001 A Warning The deuterium lamp emits UV radiation that is harmful to the eyes Always turn off the detector power before removing the lamp cover A Avertissement La lampe deuterium emettet de rayons ultraviolets qui sont dangereux pour les yeux Voulez vous etteindre le detecteur avant d enlever le couvercle de la lampe A Caution 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 A Mise en garde 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 1 Turn off the detector power 2 Open the detector front panel Tubing bracket Connector Flow cell cover cover Lamp cover Fig 34 Covers on PDA inside front panel 3 Remove the flow cell from the optical bench page 87 NOTE It is not required to disconnect the flow cell from the fluidic flow 1 e step 1 of the description of how to remove the flow cell can be omitt
100. rmed by a Dionex Service Representative Tungsten LED is flashing The lamp did not power on properly Check the Chromeleon Audit Trail for a lamp related error message If necessary replace the lamp section 1 page 92 If the LED flashes again there may be a bad connection between the lamp power supply and the lamp Contact Dionex Service for assistance NOTE The PDA 3000 electronics cannot be serviced by users All repairs of the electronics components must be performed by a Dionex Service Representative Power LED is flashing If the Power LED starts flashing the first time the deuterium lamp is turned on the detector failed the start up routine Follow the steps below to resolve the problem 1 Remove the cell from the optical bench section 6 2 4 page 2 In Chromeleon press F8 to display the Commands dialog box and select UV Operating Instructions Page 69 UltiMate 3000 Series Photodiode Array Detector 3 Select Autozero and click Execute to run the autozero routine If this corrects the problem the Power LED will stop flashing and you may replace the cell in the optical bench and resume normal operation If the Power LED continues flashing go on to step 4 4 Check the deuterium lamp intensity page 55 The intensity reading should be above 10 million counts for an analytical or semipreparative cell or above 3 million counts for a semi micro cell If the reading is acceptable and the Power L
101. rray Detector Example Chromatogram Selecting the Sample Wavelength Reference Wavelength and Reference Bandwidth Fig 28 page 51 shows the spectrum of caffeine The operating conditions are Sample wavelength 272 nm Bandwidth 5 nm Reference wavelength 325 nm Reference bandwidth 51 nm These settings calculate the absorbance by the following equation avg I 300 to 350 AU log offset in AU at autozero at 272 nm avg 270 to 274 Where Ix Light intensity Offset Absorbance offset at autozero 1200 1102 _4 Bandwidth 5 nm ri 270 nm to 274 nm 1000 250 Hi n 300 nm to 350 nm H Reference Bandwidth 51 nm y y 272 nm 325 nm Sample Wavelength Reference Wavelength Fig 28 Caffeine Spectrum Operating Instructions Page 51 UltiMate 3000 Series Photodiode Array Detector 4 3 8 Bunch Width The bunch width setting determines how many nanometers are averaged when collecting 3D data The default is 1 nm Selecting a bunch width above 1 nm will reduce the required data storage by approximately the reciprocal Do not select a bunch width when the spectrum of the compound has a fine structure the bunch width will reduce the spectral resolution 4 3 9 Step Chromeleon automatically selects the appropriate step setting Therefore it is not necessary for users to select a step setting A step is the time interval be
102. rray Detector Operating Instructions 10 Index 2D Data Single Wavelengths cc 10 ID Dat sad 4er nat dt Nes 10 Bunch Width Selection 54 Reducing Data File Size 55 Step Time Selection 55 A Absorbance Calculation 53 Active Reference Mode 51 Selecting sert terne ra 51 76 Tune Offs lus rennes Nr 51 Air Bubbles Pr v ntinesisnimnsinnniRn nent REMOVINZ lede nede Air Conditioning Ambient Temperature Fluctuations 51 Analog Output Connectors cesses 10 60 Analog Outputs ccecceccessesceeseeseeseeneeneeneeeseens 29 Analytes unknown cccecceseeseeseeseeeeeeseeeeeseens 49 Analytical Flow Cell 18 Audit Trail cccccccccescecsecessseeesseeeene 13 57 62 Automated Control ccccccceccesseeeeeesseeees 38 39 AV CLAS rendre ne R 44 46 Definitionen en SSR ENEDES HESS SE 55 Guidelines for Selecting 55 B Backpressures rrene ren rr hennes 34 Slow Increase 85 Sudden Increase 1 W u u ssseverrerereersenserersnnere 85 Backpressure Line 74 Bandwidth sssssssumamnn 44 46 D finitons rene me nee 50 Setting is OO NATTOW 75 Baseline Dr sadel ikee Baseline Noise CAUSES sisi ia Pr e Effect of Rise Time on 47 Reducingssc inner 51 82 Bunch W
103. s such as sulfuric acid and nitric acid or a mixture of hexane ethyl actate and methanol Swelling or attack by concentrated acids is not a problem with brief flushing procedures e Do not use PEEK tubing that is stressed bent or kinked e During operation the lamp and the surrounding parts become extremely hot and remain so for some time after the detector is turned off To avoid possible injury allow sufficient time for the lamp to cool before performing any maintenance or repair work e The deuterium lamp emits UV radiation that is harmful to the eyes Therefore avoid looking directly into the light source Always turn off the detector before exchanging the lamp e Use original Dionex spare parts only Substituting non Dionex parts or using non Dionex accessories may impair the performance of the instrument e Do not use the detector in ways other than those described in this manual Page 4 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 1 2 3 Consignes G n rales de S curit Veuillez noter Avant de commencer utiliser l instrument assurez vous que vous vous tes familiaris s avec le contenu de ce manuel Observez les tiquettes d avertissement sur l appareil et r f rez vous aux sections correspondantes dans ce mode d emploi Veuillez observer les consignes g n rales de s curit suivantes lorsque vous utilisez l instrument ou que vous proc dez des op rations de maintenan
104. s kit analytical cell 6080 2410 including capillary with tubing and fitting Outlet fluidics kit semi micro cell 6080 2411 including capillary with tubing and fitting Outlet fluidics kit semipreparative 6080 2412 cell including capillary with tubing and fitting 6 2 1 Liquid Leaks NOTE Periodically check all tubing and fittings and replace as necessary section 4 4 page 55 Tubing and fitting components may eventually become loose and leak or pinched off and plugged The inlet tubing of the analytical and semi micro cells cannot be replaced If a leak at the flow cell inlet for example cannot be eliminated by tightening the fitting replace the entire cell section 6 2 4 page 87 If you have located the source of a leak tighten or replace all liquid line connections first If the cell is leaking check that the backpressure on the cell does not exceed the specification section 6 2 6 page 91 Wipe up all liquid and dry the leak sensor before resuming operation If the cell leaks after you resume operation replace it section 6 2 4 page 87 Operating Instructions Page 85 UltiMate 3000 Series Photodiode Array Detector 6 2 2 Cleaning the Flow Cell Film deposits on the flow cell windows may cause excessive baseline noise or high absorbance offset 1 Pump methanol through the cell for 20 to 30 minutes at 1 0 mL min 2 Pump DI deionized water through the cell
105. semi micro cells 6080 2423 Capillary TCC PDA 0 5 mm ID PEEK for semipreparative cells 6080 2424 Cell inlet or outlet tubing PEEK for semipreparative flow cell 6080 2406 Cell outlet tubing PEEK for analytical semi micro flow cell 6080 2401 Cell outlet tubing stainless steel for analytical semi micro flow cell 6080 2403 Deuterium lamp 6080 2001 Female 12 pin connector RM3 81 6080 9010 Fitting PEEK 1 16 one piece fingertight 2 fittings 6720 0072 Fitting stainless steel 1 16 screw and ferrule 6 fittings 6822 0012 Flow cell cover 6080 1210 Flow cell window 6080 1201 Flow cell windows replacement kit including 6080 1200 Windows replacement tool 2 flow cell windows 2 window seals Fuses Kit including 4 0 A fast blow 5 x 20 mm fuse 10 fuses 6080 9001 6080 1211 Outlet fluidics kit analytical cell including capillary with tubing and fitting 6080 2410 Outlet fluidics kit semi micro cell including capillary with tubing and fitting 6080 2411 Outlet fluidics kit semipreparative cell including capillary with tubing and 6080 2412 fitting Packaging box 5035 8900 Reducing union fitting for analytical semi micro flow cell PEEK 6080 2101 Reducing union fitting for analytical semi micro flow cell SST 6080 2102 Screw driver mini for Relay TTL connector 6080 1285 Shipping container PDA 5035 8900 Tungsten lamp 6080 2002 Twisted wire assembly 2 m 8 ft for relay TT
106. side Drive 541 Lakeside Drive Sunnyvale CA 94088 3603 Sunnyvale CA 94088 3603 USA USA Test report no USA IC 09972699 008 Client Reference Art Khalig Tested to JL 61010 1 2004 CAN CSA C22 2 61010 1 2004 Certified Product Analyzer License Fee Units Addition Model Designation PDA 3000 Rated Voltage AC 100 120 220 240V 50 60Hz Signatures Date of Issue day mo yr 31 01 2007 I Sud Vo President QA Certification Officer Page II Operating Instructions UltiMate 3000 Series Photodiode Array Detector Table of Contents 1 Introduction s EL randers 1 1 1 How to Use This Mantal iiaeie ere tte rame tentes des 1 1 2 Safety Information sac nas lent 2 1 2 1 Symbols on the Instrument and in the Manual u ssnsensereeresesseree rener rreee 2 1 2 2 Gener l Safety Precautions ccccccsccesssseeesseeeessceesteeeeseeeeetecesseeeeseeeesteeeeseeens 3 1 2 3 Consignes G n rales de S curit 5 1 3 Product OVERVIEW en rene en Mahler mental erre rte niis de 7 1 4 Theory of Photodiode Array Detection Wu Xu u X sssseueeusereersersererereenen seeren eee ennen 8 PA DITA aO a a EEEE E 11 2 1 Pront KE TITS A ind dete Hin eee A eee ae ieee 11 2 2 Inside Front Panel oie ns Rem ae stresse lise dec 13 2 3 Optical Systemene kee eich dit e E I en ee 14 2 4 FONCIER en Re EE A sn einen eurent 15 2 5 Rear Panel ireen nn TN vacate eae re teen Een ane et ete 19 2 6 TSCA eS CNS OL EN nent Seta ES ie tense i
107. sor cannot detect the filter wheel position Thus if this is the only error reported you may continue operation and defer troubleshooting if desired To troubleshoot 1 Turn off the PDA 3000 power for 30 seconds and then turn it on again 2 Ifthe error message appears again check the deuterium lamp intensity page 55 The intensity reading should be above 10 million counts for an analytical or semipreparative cell or above 3 million counts for a semi micro cell If the reading is acceptable resume normal operation If the reading is too low see section 5 7 page 75 3 Ifthe error message appears again there may be a faulty connection to the filter wheel sensor Contact Dionex Service for assistance NOTE The PDA 3000 electronics cannot be serviced by users All repairs of the electronics components must be performed by a Dionex Service Representative A Invalid rise time Valid rise times at 20 Hz 0 05 0 1 0 2 0 5 1 0 and 2 0 To troubleshoot This message appears if you enter a rise time setting that is invalid for a data collection rate of 20 Hz Select a valid rise time Operating Instructions Page 65 UltiMate 3000 Series Photodiode Array Detector A Invalid step for the 3DFIELD Valid steps are 0 05 0 1 0 2 0 4 0 5 1 2 and 4 To troubleshoot This message appears if you enter an invalid step setting Chromeleon automatically selects the step value that is the inverse of the data collec
108. ss the LED is lighted If an error occurs the LED flashes and an error message is logged in the Chromeleon Audit Trail UltiMate 3000 Phot RUN DEUTERIUM TUNGSTEN POWER CI lt Power switch Fig 3 PDA 3000 Photodiode Array Detector LED LED Status Function Run Lighted Data is being acquired by Chromeleon Flashing The leak sensor in the drip tray was triggered Off Data is not being acquired by Chromeleon Deuterium Lighted The deuterium lamp is on Flashing A command was issued to turn on the deuterium lamp but the lamp failed to turn on section 5 3 page 70 If a subsequent attempt to turn on the lamp is successful the LED will automatically stop flashing Off The deuterium lamp is off Operating Instructions Page 11 UltiMate 3000 Series 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 section 5 3 page 70 If a subsequent attempt to turn on the lamp is successful the LED will automatically stop flashing Off The tungsten lamp is off Power Lighted The detector power is on Press the Power switch for on off control of the detector Flashing The detector failed the start up routine section 5 2 page 69 Off The detector power is off Press the Power switch for on off con
109. sult in minor or moderate injury Important Indicates that the function or process of the instrument may be impaired Operation does not constitute a hazard Page 2 Operating Instructions UltiMate 3000 Series Photodiode Array Detector Messages d avertissement en frangais VAN Danger Signale une situation de danger imm diat qui si elle n est pas vit e entra nera des blessures graves mortelles A Avertissement Signale une situation de danger potentiel qui si elle n est pas evit e pourrait entra ner des blessures graves mortelles A Mise en garde Signale une situation de danger potentiel qui si elle n est pas vit e pourrait entra ner des blessures mineures mod r es galement utilis pour signaler une situation ou une pratique qui pourrait gravement endommager l instrument mais qui n entra nera pas de blessures Informational messages also appear throughout this manual These are labeled NOTE Notes call attention to certain information They alert users to an unexpected result of an action suggest how to optimize instrument performance etc 1 2 2 General Safety Precautions When working with analytical instrumentation you should know the potential hazards of using chemical solvents NOTE Before initial operation of the detector make sure that you are familiar with the contents of this manual Observe any warning labels on the device and refer to the related sections in th
110. sure not to twist the end of the flow cell inlet and outlet tubings when connecting them from to the liquid line connections Preferably use a tool to hold the union fitting while you remove or install any connections Fig 29 Union fitting Removing the Flow Cell from the Optical Bench When the flow cell is removed light may emit from the opening to the right of the flow cell Looking directly into the light source will cause immediate injury to your eyes Remove the flow cell from the optical bench before replacing the cell windows section 6 2 5 installing a new cell or inspecting the cell for leaks or obstructions 1 Open the front panel door 2 Disconnect the tubing connected to the flow cell inlet and outlet 3 Remove the two knurled head screws on the flow cell cover and then remove the cover Fig 4 page 13 4 Analytical or semi micro cell Remove the two knurled head screws on the tubing bracket to remove the bracket from the lamp cover Fig 30 5 Remove the flow cell inlet tubing from the tubing guide in the lamp cover Fig 30 Operating Instructions Page 87 UltiMate 3000 Series Photodiode Array Detector 6 Squeeze the handle of the flow cell and pull it out of the optical bench Fig 30 Removing the Flow Cell from the Optical Bench Flow cell cover not shown Installing a New Flow Cell Follow the descriptions how to install a flow cell in section 3 6 gt page 29
111. t it into the 4 pin bulkhead connector on the side wall Route the wires through the wire guide in the optical bench Fig 35 page 93 Replace the lamp cover Route the wires through the guides on the lamp cover inside Fig 36 page 94 Do not pinch the Vis lamp connector wires under the lamp cover Replace the flow cell and flow cell cover page 31 Close the detector front door Turn on the detector power Start the Chromeleon server Reset the lamp lifetime page 55 NOTE Before resuming routine operation allow 20 to 30 minutes for the lamp to stabilize Page 96 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 6 4 Replacing the Main Power Fuses Description Part No Fuse 4 0 amp fast blow IEC 127 Fuses kit 6080 9001 A Danger HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the PDA 3000 A Danger HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du PDA 3000 Before replacing the fuses turn off the detector Be sure to disconnect the power cord from its source The fuse holder is part of the main power receptacle gt Fig 37 page 97 Using a small screwdriver or your fingernails push the lock upward to release it The fuse holder will pop out slightly when the lock is released Pull the fuse holder straight out of the compartment
112. t solutions salines sont toxiques Informez vous des propri t s toxicologiques de toutes les phases mobiles que vous utilisez e Les propri t s toxicologiques de nombreux chantillons peuvent tre mal connues Au moindre doute concernant un chantillon traitez le comme s il contenait une substance potentiellement dangereuse Operating Instructions Page 5 UltiMate 3000 Series Photodiode Array Detector e Portez des lunettes de protection lorsque vous manipulez des phases mobiles ou que vous utilisez l instrument Une installation permettant de se laver les yeux ainsi qu un lavabo doivent se trouver proximit du syst me Si une phase mobile quelle qu elle soit gicle dans les yeux ou sur la peau lavez la zone affect e et consultez un m decin e D barrassez vous de tous les d chets de phase mobile de mani re cologique conform ment la r glementation en vigueur au niveau local Emp chez imp rativement l accumulation de solvants inflammables et ou toxiques Suivez un programme d limination des d chets r glement et approuv Ne jetez jamais de solvants inflammables et ou toxiques dans le syst me municipal d vacuation des eaux us es e Utilisez uniquement des solvants qualit HPLC et des solutions salines compatibles avec les mat riaux expos s phase mobiles e Dans un syst me UltiMate 3000 certaines composantes sont en PEEK Bien que ce polym re pr sente une excellente r sistance chimique la
113. tandard Accessories for PDA 3000 5080 8910 Screw driver mini for Relay TTL connector 6080 1285 Fuse 4A fast blow 162VA 5 x 20 mm included in 6080 9001 12 pin relay TTL connector 6080 9010 Tubing and Tee piece for waste fluid included in connection 6000 5001 Assortment box for accessories 6000 0043 USB cable type A to type B USB 2 0 5m 6911 0002 ae 8 1 2 Flow Cells Flow cells must be ordered separately Cells are shipped with outlet fluidics backpressure line and capillary to the column compartment and fittings Description Analytical PEEK flow cell assembly 6080 0200 Analytical stainless steel flow cell assembly 6080 0210 Semi micro PEEK flow cell assembly 6080 0220 Semi micro stainless steel flow cell assembly 6080 0230 Semipreparative PEEK flow cell assembly 6080 0240 Operating Instructions Page 101 UltiMate 3000 Series Photodiode Array Detector 8 1 3 Spare Parts and Consumables 12 pin relay TTL connector 6080 9010 Analytical reducing union fitting PEEK 6080 2101 Analytical reducing union fitting 6080 2102 Assortment box for accessories 6000 0043 Backpressure line 2 m 0 25 mm ID with fitting 6080 2413 Capillary TCC PDA 0 25 mm ID stainless steel for analytical cells 6080 2400 Capillary TCC PDA 0 25 mm ID PEEK for analytical cells 6080 2421 Capillary TCC PDA 0 13 mm ID PEEK for semi micro cells 6080 2422 Capillary TCC PDA 0 13 mm ID stainless steel for
114. ted standards pages I and II 1 2 1 Symbols on the Instrument and in the Manual The table below shows the symbols used on the instrument Symbol Description w Alternating current Courant alternatif Power supply is on L instrument est mis en circuit Power supply is off L instrument est mis hors circuit the instrument against damage R f rez vous au ce manuel pour viter un risque de blessure l op rateur et ou de prot ger l instrument contre des dommages Harmful radiation Avoid looking directly into light sources Rayons dangereux Ne regardez pas directement la lumi re WEEE Waste Electrical and Electronic Equipment label For more information refer to the WEEE Information section in the manual binder tiquette de WEEE Waste Electrical and Electronic Equipment Pour plus d information r f rez vous la section WEEE Information dans ce fichier A Refer to the operating instructions to prevent risk of harm to the operator and to protect At various points throughout the manual messages of particular importance are indicated by certain symbols VAN Danger Indicates an imminently hazardous situation which if not avoided will result in death or serious injury A Warning Indicates a potentially hazardous situation which if not avoided may result in death or serious injury A Caution Indicates a potentially hazardous situation which if not avoided may re
115. ting Instructions UltiMate 3000 Series Photodiode Array Detector 10 Select the operating parameters section 4 3 page 44 Go to the Pump tab and turn on the pump Set the flow rate and mobile phase composition Click Acq On to begin manual data acquisition Click Acq Off to stop manual data acquisition after the desired run time Data collected during the run may be saved to a sequence To retrieve the data select the assigned sample name within the sequence 4 2 2 Automated Control A PGM file is a list of time precise control commands created by the user for automated operation of the PDA 3000 PGM files can be created automatically with the help of the PGM Wizard or manually by editing an existing PGM file 1 Start the Chromeleon Server by double clicking the Server Monitor icon on the taskbar 2 Start Chromeleon by selecting Start gt Programs gt Chromeleon gt Chromeleon The main window and the Browser will appear Creating a New PGM File Careful selection of the data collection rate rise time and other operating parameters will optimize the performance of the PDA 3000 Before creating a PGM file you may want to review section 4 2 3 page 42 for a description of these parameters how they interact with each other and some guidelines for their selection 1 Select File gt New A dialog box appears Select Program File and click OK The initial Program Wizard screen is displayed
116. tion rate In future accept the value selected by the software Only advanced users should override the step setting selected by Chromeleon Selecting an inappropriate step setting may cause loss of sensitivity skipped data points and other problems Leak sensor error To troubleshoot Locate the source of the leak First tighten or replace all liquid line connections If the cell is leaking check that the backpressure on the cell does not exceed the specification section 6 2 6 page 91 Wipe up all liquid and dry the leak sensor before resuming operation If the cell leaks after you resume operation replace it gt section 6 2 4 page 87 D Not enough light to perform operation To troubleshoot Follow the troubleshooting steps in Section 5 7 page 75 Over temperature error To troubleshoot The fan that cools the optical bench may have malfunctioned or a component on the lamp supply board may have failed Turn off the PDA 3000 power and contact Dionex Service for assistance NOTE Do not attempt to service the PDA 3000 electronics components All repairs of the electronics components must be performed by a Dionex Service Representative Page 66 Operating Instructions UltiMate 3000 Series Photodiode Array Detector PDA is running a calibration or diagnostic function Not ready to accept this command To troubleshoot Wait until the calibration procedure or diagnostic rout
117. trol of the detector Table PDA 3000 Front Panel LEDs Page 12 Operating Instructions UltiMate 3000 Series Photodiode Array Detector 2 2 Inside Front Panel Grasp the PDA 3000 front panel by the sides and pull it straight off to access the inside front panel 5 2 3 4 Fig 4 PDA 3000 Inside Front Panel No Description 1 Slots in the enclosure to thread the flow cell capillaries to the outside 2 Flow cell cover The flow cell cover protects the cell from dust ambient light fluctuations in ambient temperature and vibration Note that the PDA 3000 is shipped without a flow cell Flow cells must be ordered separately 3 Lamp cover The lamp cover enhances the thermal stabilization of the optical bench The deuterium and or tungsten lamp is installed behind the cover page 91 4 Leak sensor page 20 5 Tubing bracket The bracket holds the flow cell inlet tubing with the heat exchanger Operating Instructions Page 13 UltiMate 3000 Series Photodiode Array Detector 2 3 Optical System Fig 5 is a schematic of the PDA 3000 optical system Light from the tungsten lamp is focused through an opening in the internal structure of the deuterium lamp Light from the tungsten and deuterium lamps is then focused through the flow cell by the source lens After exiting the cell the light passes through the spectrograph lens to the filter paddle and is focused into the slit Th
118. tween two successively stored data points The smaller the step is the more data points are recorded and in general the more precise is the analytical results However because collecting more data points requires more storage capacity the step setting sometimes represents a compromise between the amount of information collected and the file size Chromeleon automatically selects the step value that is the inverse of the data collection rate selected by the user For example if the data collection rate is 5 0 Hz the software sets the step to 0 2 second The following table indicates the step setting automatically selected for each data collection rate Data Collection Rate Step Hz seconds 0 25 4 0 0 5 2 0 1 0 1 0 2 0 0 5 2 5 0 4 5 0 0 2 10 0 0 1 20 0 0 05 Page 52 Operating Instructions UltiMate 3000 Series Photodiode Array Detector Step Override Important This section explains how to override the step setting automatically selected by Chromeleon This information is provided for reference by advanced users only Be aware that selecting an inappropriate step setting may cause loss of sensitivity skipped data points and other problems In almost all cases the step setting selected by Chromeleon is the preferred setting However it is possible to override this setting by manually changing the step in the PGM file or on the Control panel
119. ty at 520 nm in counts per seconds Check the deuterium lamp intensity approximately every 6 months Operating Instructions Page 55 UltiMate 3000 Series Photodiode Array Detector Check that at least one lamp is turned on When a lamp is on the corresponding front panel LED Deuterium or Tungsten is lighted If necessary turn on one of the lamps from either Chromeleon or the TTL input To check the UV lamp intensity 1 In Chromeleon press F8 to display the Commands dialog box and select UV 2 Select LampIntensity The reading should be above 10 million counts for an analytical or semipreparative cell or above 3 million counts for a semi micro cell However a lamp with less intensity may work sufficiently depending on the noise level required for the application If the reading is too low follow the steps in Section 5 7 page 75 to resolve the problem e Wavelength calibration Purpose Improves wavelength accuracy in the UV range by reassigning new wavelengths to each pixel based on the emission spectrum from the deuterium lamp The results of both the initial calibration and the last calibration are stored in the calibration log You can view the results at any time 1 Verify the following conditions no solvent is flowing through the cell the background absorbance is low and there are no bubbles in the light path 2 Inthe Browser navigate to the following folder Dionex Templates Panels Dionex_LC 3
120. u touch a window clean it with isopropyl alcohol and a clean lens tissue Strong bases can etch the fused silica windows of the flow cell If the mobile phase is a base make sure the mobile phase concentration does not exceed 0 1 M If the concentration of the base is greater than 50 mM disconnect the separator column and flush the system with DI deionized water for 5 minutes at 1 0 mL min immediately after the analysis If strong base remains in the cell for 1 or 2 days the cell windows may need to be replaced section 6 2 5 page 89 Do not use a PEEK flow cell with normal phase or chlorinated solvents these solvents will damage the cell Do not use the stainless steel flow cell with low pH solutions these solutions may cause corrosion contamination and metal leaching Operating Instructions Page 15 UltiMate 3000 Series Photodiode Array Detector Analytical Flow Cell Part No Cell Cell Cell Volume of Heat Exchanger Intended Material Volume Path Inlet Tubing Flow Rate Length Range 6080 0200 PEEK 13 uL 10 mm 45 uL 0 5 to 5 0 mL min 6080 0210 316 13 uL 10 mm 20 uL 0 5 to 5 0 Stainless mL min Steel The analytical flow cell assembly Fig 6 is available in PEEK and 316 stainless steel Two built in heat exchangers one on the cell inlet tubing and one on the cell handle help stabilize the temperature of the mobile phase before it enters the cell The anal
121. um and or Tungsten LEDs are lighted 4 Wait 20 to 30 minutes for the lamps to stabilize For sensitive applications or for detector validation allow at least 2 hours After installing a new lamp allow 8 to 24 hours 4 2 Routine Operation by Chromeleon Two modes of software control are available e Direct Control section 4 2 1 With direct control you select operating parameters and commands from control panels or the Commands F8 dialog box Direct commands are executed as soon as they are entered To open the Commands dialog box open a Chromeleon control panel Select Command on the Control menu The Commands dialog box is opened You can also open this box by pressing the F8 key To display the commands and properties that are available for the detector click the sign beside UV in the left list box e Automated Control section 4 2 2 With automated control you create a program or PGM File This is a list of control commands executed in chronological order for automated operation of the detector Programs can be created automatically with the help of a software wizard or manually by editing an existing program For details about how to control the detector refer to the Chromeleon online Help and or User Manual Operating Instructions Page 35 UltiMate 3000 Series Photodiode Array Detector 4 2 1 Direct Control In the direct control mode PDA 3000 commands and operating parameters are selected fr
122. velengths are within the UV spectrum 190 to 380 nm of the deuterium lamp e Ifthe sample wavelength is 572 nm you might select a reference wavelength of 425 nm because both wavelengths are within the visible spectrum 380 to 800 nm of the tungsten lamp The active reference mode minimizes baseline drift and is ideal for gradient analyses where the baseline may shift This mode also helps compensate for fluctuations in ambient temperature caused by air conditioning NOTE When the active reference mode is selected select a reference wavelength and reference bandwidth in a quiet area of the spectrum where little absorption occurs The reference wavelength plus one half the reference bandwidth must be within the sample wavelength range selected page 39 If the data collection rate is 20 Hz the 3D sample wavelength range must be lt 310 nm see page 46 e To cancel the active reference mode enter Off as the reference wavelength The intensity reading at the time of autozero will be used as the reference intensity When running an isocratic analysis in a laboratory with stable ambient temperature operating the detector with the active reference mode turned off ensures the lowest baseline noise It also ensures that fluctuations in signal intensity in the reference wavelength do not cause additional noise Example Chromatogram Selecting the Reference Wavelength Fig 27 shows the results obtained from two different channels
123. within the same run When the reference wavelength mode is Off 1 e the active reference mode is cancelled the baseline drift is 120 HAU hour When the active reference mode is selected the baseline drift is reduced to 40 pAU hour Operating Instructions Page 49 UltiMate 3000 Series Photodiode Array Detector The operating conditions are Sample wavelength 520 nm Bandwidth 10 nm Reference bandwidth 50 nm active reference mode only Flowing water at 1 0 mL min 10 35 MPa 1500 psi Reference Wavelength Mode Off Baseline Drift 120 LAU hour mAU min Reference Wavelength Mode Active Baseline Drift 40 LAU hour mAU min Fig 27 Effect of Reference Wavelength on Baseline Drift 4 3 7 Reference Bandwidth The reference bandwidth is analogous to the conventional bandwidth of a channel The purpose of the reference bandwidth is to average several photodiode signals in a range surrounding the reference wavelength It is not necessary to select a reference bandwidth unless you enter a reference wavelength i e you select the active reference mode If you enter Off as the reference wavelength the reference bandwidth will be the same as the bandwidth Select a reference bandwidth that is narrow enough not to interfere with nearby compounds and select an area of the spectrum where the sample does not absorb Page 50 Operating Instructions UltiMate 3000 Series Photodiode A
124. 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 Page 74 Operating Instructions UltiMate 3000 Series Photodiode Array Detector Leaking flow cell Tighten fittings Also check that the backpressure on the cell does not exceed the specification section 6 2 6 page 91 If the cell continues to leak replace it section 6 2 4 page 87 Absorbance in the reference wavelength Sample absorbance in the selected reference wavelength may cause excessive baseline drift Select a reference wavelength and reference bandwidth in an area of the spectrum where little absorption occurs page 50 Dionex recommends selecting a reference wavelength 1 e active reference mode for gradient analyses and turning off the reference wavelength for isocratic analyses in a laboratory with a stable ambient temperature page 49 5 7 Deuterium Lamp Intensity Reading Too Low Light signal is not reaching the data processor Check that at least one lamp is turned on When a lamp is on the corresponding front panel LED Deuterium or Tungsten is lighted If necessary turn on one of the lamps from either Chromeleon or the TTL input Low light throughput 1 Remove the cell from the optical bench section 6 2 4 page 87 2
125. ytical cell is designed for applications with 3 to 4 mm ID separator columns and flow rates of 0 5 to 5 0 mL min Fa Cell Outlet Tubing Reducing Union Fitting a Cell Inlet Tubing Reducing Union Fitting Flow Cell Heat Exchangers Spring Clip Fig 6 Analytical Flow Cell Assembly Description PEEK Stainless Steel 6080 0200 6080 0200 P N P N Reducing union fittings 6080 2102 Cell outlet tubing 6080 2403 0 25 mm 0 010 in ID Outlet fluidics kit including 6080 2410 capillary with tubing and fitting Page 16 Operating Instructions UltiMate 3000 Series Photodiode Array Detector Semi Micro Flow Cell Part No Cell Cell Cell Path Volume of Heat Intended Flow Material Volume Length Exchanger Inlet Rate Range Tubing 6080 0220 9 mm 5 uL Up to 1 0 mL min 6080 0230 316 3 1 pL 9 mm 5 uL Up to 1 0 Stainless mL min Steel The semi micro flow cell assembly Fig 7 is available in PEEK and 316 stainless steel Two built in heat exchangers one on the cell inlet tubing and one on the cell handle help stabilize the temperature of the mobile phase before it enters the cell The semi micro flow cell is designed for applications with 2 to 3 mm ID separator columns and flow rates of up to 1 0 mL min JE Cell Outlet Tubing Reducing Union Fitting p a Cell Inlet Tubing Reducing Union Fitting ps Flow

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