Dionex PDA-100 Operator'S Manual Download Page 86

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PDA-100 Photodiode Array Detector

A-2

Doc. 031644-02 9/03

A.4 Detector

Optical System

Single-beam, reverse-optics design with concave holographic
grating

Light Sources

Deuterium lamp (30 W) for ultraviolet spectrum analysis
Tungsten lamp (15 W) for visible spectrum analysis

Photodiode Array

1024 elements

Wavelength

Range

190 nm to 800 nm

Pixel Resolution

0.7 nm

Wavelength

Accuracy

1 nm

Noise

± 10

AU with 2-second rise time, 254 nm, 4 nm bandwidth,

and flowing deionized water
± 15

AU with 2-second rise time, 520 nm, 10 nm bandwidth,

and flowing deionized water

Drift

< 500

AU/hour (after warm-up)

Linearity

> 2 AU

Analog Outputs

Four built-in analog outputs

Voltage Out

1 V output

Analog Output

Range

0.0005, 0.001, 0.01, 0.1, 0.5, 1.0, 2.0, or 3.0 AU full-scale

Control and Data

Evaluation

Provided by PeakNet 6 or Chromeleon software; communication
with the detector is via the DX-LAN interface

Summary of Contents for PDA-100

Page 1: ...PDA 100 PHOTODIODE ARRAY DETECTOR OPERATOR S MANUAL 2003 Dionex Corporation Document No 031644 Revision 02 September 2003 ...

Page 2: ...S PUBLICATION IS PROVIDED AS IS WITHOUT WARRANTY OF ANY KIND DIONEX CORPORATION DOES NOT WARRANT GUARANTEE OR MAKE ANY EXPRESS OR IMPLIED REPRESENTATIONS REGARDING THE USE OR THE RESULTS OF THE USE OF THIS PUBLICATION IN TERMS OF CORRECTNESS ACCURACY RELIABILITY CURRENTNESS OR OTHERWISE FURTHER DIONEX CORPORATION RESERVES THE RIGHT TO REVISE THIS PUBLICATION AND TO MAKE CHANGES FROM TIME TO TIME I...

Page 3: ... 1 3 About This Manual 1 5 1 3 1 Safety Messages and Notes 1 6 1 4 Safety Labels 1 8 2 Description 2 1 Front Panel 2 1 2 2 Inside Front Panel 2 3 2 3 Optical System 2 4 2 3 1 Flow Cell 2 6 2 4 Electronics 2 7 2 5 Rear Panel 2 10 3 Operation and Maintenance 3 1 Operating Guidelines 3 1 3 1 1 Mobile Phases 3 1 3 1 2 Solvent Delivery System 3 2 3 2 Getting Started 3 4 ...

Page 4: ...4 3 Noisy Baseline 4 3 4 4 Drifting Baseline 4 6 4 5 Lamp Does Not Light or Lamp LED Is Flashing 4 7 4 6 Deuterium Lamp Intensity Count Too Low 4 7 4 7 Wavelength Calibration Fails 4 8 4 8 Wavelength Verification Fails 4 9 4 9 Faulty DX LAN Communication 4 10 4 10 No Spectra Collected 4 10 4 11 Low Spectral Resolution 4 10 4 12 Peaks Too Large or Small 4 11 4 13 Poor Peak Shape 4 12 4 14 Error Mes...

Page 5: ...5 4 Removing the Flow Cell 5 3 5 5 Replacing the Flow Cell Windows 5 4 5 6 Replacing the Flow Cell 5 5 5 7 Replacing the Deuterium Lamp 5 6 5 8 Replacing the Tungsten Lamp 5 9 5 9 Replacing the Main Power Fuses 5 11 A Specifications A 1 Physical A 1 A 2 Environmental A 1 A 3 Electrical A 1 A 4 Detector A 2 A 5 Flow Cells A 3 A 6 Heat Exchangers A 3 B Installation B 1 Facilities Required B 1 ...

Page 6: ...or iv Doc 031644 02 9 03 B 2 Unpacking B 1 B 3 Installation B 2 B 3 1 Power B 2 B 3 2 Flow Cell B 3 B 3 3 Waste Line B 5 B 3 4 Detector Output Analog B 5 B 3 5 Relay TTL Control B 6 B 3 6 DX LAN Interface B 8 C Reordering Information ...

Page 7: ...to perform extractions for runs that do not require spectral data and it conserves disk space Key PDA 100 features include Deuterium and tungsten lamps ensure low baseline noise high signal intensity and applications flexibility in the wavelength range from 190 nm to 800 nm A 1024 element photodiode array optimizes spectral resolution A built in holmium oxide filter verifies wavelength calibration...

Page 8: ...llows an accurate assessment of peak identity purity and quantitation in a single run Software support for PDA detectors includes peak purity and spectral library search functions to help determine peak homogeneity and identity 1 2 1 Advantages of Photodiode Array Detection PDA detectors are useful in both research and quality assurance laboratories In the research laboratory the PDA provides the ...

Page 9: ...ectra throughout the peak at all wavelengths Positive peak identification In liquid chromatography peak identification is usually based on relative retention times When a PDA detector is used spectra are automatically collected as each peak elutes The PDA software compares the spectra with those stored in a library to determine the best fit matches this method increases the likelihood of correctly...

Page 10: ...PDA 100 Photodiode Array Detector 1 4 Doc 031644 02 9 03 Figure 1 1 Overlay of Pyrene and an Impurity Figure 1 2 Spectra of Pyrene and an Impurity Impurity Pyrene Impurity Pyrene ...

Page 11: ...nce Presents an overview of PDA 100 operation as well as guidelines for optimizing detector performance Lists routine preventive maintenance procedures Chapter 4 Troubleshooting Lists problems that may occur along with step by step instructions for resolving them Chapter 5 Service Contains step by step instructions for routine service and parts replacement procedures Appendix A Specifications List...

Page 12: ...e and are accompanied by icons as shown below Indicates an imminently hazardous situation which if not avoided will result in death or serious injury Indicates a potentially hazardous situation which if not avoided may result in death or serious injury Indicates a potentially hazardous situation which if not avoided may result in minor or moderate injury Indicates that the function or process of t...

Page 13: ...ée pourrait entraîner des blessures graves à mortelles Signale une situation de danger potentiel qui si elle n est pas évitée pourrait entraîner des blessures mineures à modérées Également utilisé pour signaler une situation ou une pratique qui pourrait gravement endommager l instrument mais qui n entraînera pas de blessures Bedeutet unmittelbare Gefahr Mißachtung kann zum Tod oder schwerwiegenden...

Page 14: ...cate that the PDA 100 is in compliance with the following standards EN 61010 1 1993 safety CAN CSA C22 2 No 1010 1 92 safety UL 3101 1 10 93 safety EN 50082 1 1992 susceptibility and EN 55011 1991 emissions These symbols appear on the PDA 100 or on PDA 100 labels Alternating current Protective conductor terminal Power supply is on Power supply is off ...

Page 15: ...indicates that an error occurred for an explanation check the Audit Trail in PeakNet 6 or Chromeleon Figure 2 1 PDA 100 Front Panel LED LED Status Function Run Lighted Data is being acquired by the host computer Flashing An alarm was activated for example the leak sensor in the drip tray may have been triggered Off Data is not being acquired by the host computer Deuterium Lighted The deuterium lam...

Page 16: ... on see Section 4 5 Off The tungsten lamp is off Power Lighted The detector power is on Press the Power switch to turn the detector on and off Flashing The detector failed one of the electrical checks or optical checks performed during the power up sequence see Section 4 15 1 Off The detector power is off Press the Power switch to turn the detector on and off LED LED Status Function ...

Page 17: ...he cell tubing connections are not immediately apparent To prevent damage to detector components the bottom of the optical bench contains a built in leak tray A sensor in the sump of the leak tray responds to changes in the index of refraction when wet If the leak sensor is activated it triggers an alarm in the detector and the front panel Run LED begins flashing see Figure 2 1 In addition the lea...

Page 18: ...flow cell by the source lens After exiting the cell the light passes through the spectrograph lens to the filter paddle and is focused into the slit The light then passes through the slit to the grating where it is separated into its component wavelengths and diffracted to the photodiode array Each diode measures a narrow portion of the spectrum Figure 2 3 PDA 100 Optical System Grating Slit Flow ...

Page 19: ... The cell has a flat window on each side Spectrograph Lens Receives the light from the flow cell and focuses it onto the slit Filter Paddle 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 wi...

Page 20: ...w Cell Cell Path Length Cell Volume Heat Exchanger Volume PEEK P N 056346 10 mm 13 µL 20 µL Stainless Steel P N 056126 10 mm 13 µL 9 µL Do not touch the cell windows If you touch a window clean it with denatured alcohol and a clean lens tissue Do not use the PEEK flow cell with normal phase or chlorinated solvents these solvents will damage the cell Do not use the stainless steel flow cell with hi...

Page 21: ...par l utilisateur Toute réparation doit être effectuée par un personnel qualifié utilisant des procédures correctes de décharge électrostatique Halten Sie sich von der Elektronik des PDA 100 fern Die Elektronik kann nicht vom Anwender gewartet werden Falls ein Service erforderlich ist ist dieser von qualifiziertem Personal durchzuführen Dabei müssen die geeigneten Verfahren zur elektrostatischen E...

Page 22: ...ly to the preamplifier The preamp gain is automatically adjusted to compensate for system variables such as lamp intensity Analog to digital conversion of the signal occurs on the Preamp card Preamp output is directed to the Data Processing card SHOCK HAZARD Components used to ignite and operate the deuterium lamp are at high potentials DANGER D ÉLECTROCUTION Les composants utilisés pour allumer e...

Page 23: ...sing card Four BNC connectors on the card provide the analog recorder outputs Select the output scale polarity baseline offset and filter rise time from PeakNet 6 or Chromeleon In addition the Data Processing card provides the digital signal processing and conversion to log ratios when absorbance is measured ...

Page 24: ...CK REPLACE ONLY WITH SAME TYPE AND RATING OF FUSE WARNING DUAL FUSE INPUTS REMOVE POWER CORD BEFORE SERVICING H3 15A 250V XXXXXXXX TUV MODEL PDA 100 INPUT 100 240V 50 60Hz 1 5A SERIAL NUMBER 035779 05 Made in U S A Dionex Corporation Sunnyvale California 94086 An alternative license is available on reasonable terms to practice any of the foregoing methods of use which can be praticed without infri...

Page 25: ...le STROMSCHLAGGEFAHR Zur Vermeidung von elektrischen Schlägen ist eine geerdete Steckdose zu verwenden Das Gerät darf nicht ohne Erdung betrieben bzw an Wechselstrom angeschlossen werden Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung Stellen Sie sicher daß sich die Steckdose nahe am Gerät befindet und leicht zugänglich ist For continued protection against risk of fire or shock repl...

Page 26: ...art of a PGM file see Section 3 3 2 or controlled manually through a control panel in the software The Relay outputs can be programmed to switch any low voltage control The switched current must be less than 200 mA and 42 V peak For installation instructions for the Relay and TTL connectors refer to Section B 3 5 DX LAN Connector The 10BASE T DX LAN RJ 45 connector on the rear panel allows communi...

Page 27: ...emicals and ASTM Type I or better filtered deionized water Degas all mobile phases before use and maintain them in a degassed state Mobile phase pH affects not only the retention time of the separation but the sample absorbance and the background absorbance of the mobile phase If an analysis employs chemical suppression and compound detection techniques compare the UV cutoff of the mobile phase be...

Page 28: ...manual All materials in the solvent delivery system must be fully compatible with the mobile phases required for the analysis For example IC and BioLC analyses frequently use mobile phases with extremes of pH or with high salt concentration A PEEK pumping system and PEEK flow cell are required when running these mobile phases because the presence of stainless steel in the flow path would contamina...

Page 29: ...inue flushing for several hours 5 Flush the system with deionized water at 1 0 mL min for 15 to 20 minutes 6 Reinstall the column and the suppressor if removed and equilibrate the system before resuming operation 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...

Page 30: ...erium lamp is turned on the detector checks the wavelength to pixel assignment if a problem is detected the Power LED will flash If this occurs flush the flow cell with deionized water or methanol and then turn off the detector power briefly Turn on the power again and verify that the Power LED is lighted but is not flashing NOTE If solvent remains in the flow cell for an extended period it may fo...

Page 31: ...r selects PDA 100 operating parameters and commands from a control panel in the software Commands are executed as soon as they are entered and parameters can be modified at any time during manual data acquisition NOTE This section provides a brief overview of detector control For complete operating instructions refer to the PeakNet 6 or Chromeleon online Help or user s manual Summary of control pa...

Page 32: ...n to begin manual data acquisition 8 Click the Acquisition On Off toolbar button to stop manual data acquisition after the desired run time 9 Data collected during the run may be saved to a sequence To retrieve the data select the assigned sample name within the sequence Figure 3 1 PDA 100 2D Control Panel Example Pump Pressure Limits Chromatogram s Acquisition On Off Detector Signals for UV1 and ...

Page 33: ...3 Operation and Maintenance Doc 031644 02 9 03 3 7 Figure 3 2 PDA 100 3D Control Panel Example ...

Page 34: ...zero Adjusts the output to zero Recorder_Range Sets the full scale recorder output range Offset_Level Sets the offset applied to the recorder output Reference_Mode Reports the reference mode RefWavelength 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 RefBandwidth Sets the bandwidt...

Page 35: ...6 or Chromeleon online Help or user s manual Summary of programmed control 1 Start PeakNet 6 or Chromeleon 2 Create a new PGM file see the following section or modify an existing program 3 Create a new sequence or modify an existing sequence 4 Select one of the PDA 100 default control panels DIONEX_PUMP_PDA_AUTOSAMPLER PAN the 2D control panel monitors chromatograms of up to five signals see Figur...

Page 36: ...a Program Wizard to facilitate the creation of new PGM files To activate the Wizard go to the File menu and select the New command A dialog box appears 2 Select Program File and click OK The initial Program Wizard screen is displayed 3 Select the Timebase where the program will run 4 Click the Next button to continue ...

Page 37: ...e displayed before the PDA 100 screens If necessary click the Next button in each screen for another device until the following screen is displayed 5 Select the data Acquisition Time 6 Check or clear the 3DFIELD check box to indicate whether 3D data will be collected 7 Check or clear the check box for each 2D single wavelength channel to be collected 8 Click Next ...

Page 38: ...een is displayed 9 Select the Data Collection Rate and the Rise Time NOTE The PDA 100 performance can be optimized by careful selection of the data collection rate rise time and other operating parameters For details refer to Section 3 4 10 Select the Lamp status 11 Click Next ...

Page 39: ...erence Wavelength plus one half the Reference Bandwidth cannot be outside the 3D Wavelength range If the values are outside this range the Reference Wavelength setting will default to the longest wavelength possible given the bandwidth In the screen shot above the selected parameters are acceptable because 750 nm plus 25 nm one half of 50 nm is less than 800 nm 13 Click Next ...

Page 40: ...ings selected for UV_VIS_1 through UV_VIS_4 apply to both analog outputs and digital outputs UV channel 1 analog output 1 UV2 analog output 2 etc Specify the Recorder Range in mAU per volt for each analog output that will be collected NOTE When the Reference Wavelength is Off the Reference Bandwidth is not used and the sample wavelength and sample bandwidth are used as reference parameters 15 Afte...

Page 41: ...ial Chemical compatibility Rise time Peak resolution sensitivity baseline noise Data collection rate Peak resolution disk space Sample wavelength Sensitivity linearity Sample bandwidth Sensitivity vs baseline noise Reference wavelength Baseline drift Reference bandwidth Baseline noise baseline drift Step Baseline noise rise time data collection rate disk space Bunch width Spectral resolution peak ...

Page 42: ...ak of interest A longer rise time allows more averaging of the signal and results in less short term noise see Figure 3 3 However a rise time that is too long may result in reduced peak heights and asymmetric peak shapes When set correctly the rise time significantly reduces baseline noise but reduces peak height only slightly Figure 3 3 Effect of Rise Time on Baseline Noise 0 0100 0 0000 0 0100 0...

Page 43: ...er peak is recommended If all peaks are relatively wide select a slower data collection rate 1 0 Hz for example If any peaks of interest are less than a few seconds select a faster data collection rate 5 0 Hz for example If the data collection rate is too slow the start and end points of peaks are not accurately determined However if the collection rate is too fast data files may occupy excessive ...

Page 44: ...detector can run five separate wavelengths without being required to collect spectra Collecting individual wavelengths instead of the spectra offers two advantages it saves disk space when 3D data is not required and it eliminates the need to perform extractions for runs that do not require spectral data If little is known about the analytes in the sample collect spectra over the full wavelength r...

Page 45: ...width reduces baseline noise but may also reduce peak height For narrow spectral peaks select narrow bandwidths Example Chromatogram Selecting the Bandwidth Figure 3 4 illustrates how selecting a wide bandwidth for both the sample and reference reduces noise by averaging over a wavelength range The operating conditions are Sample wavelength 254 nm Reference wavelength Off Flowing water at 1 0 mL m...

Page 46: ...the sample wavelength is 272 nm you might select a reference wavelength of 325 nm both wavelengths are within the UV spectrum of the deuterium lamp 190 nm to 380 nm Active reference mode minimizes baseline drift and is ideal for gradient analyses where the baseline may shift Active mode also helps compensate for fluctuations in ambient temperature caused by air conditioning NOTE When active refere...

Page 47: ...r when a reference wavelength active mode is selected baseline drift is reduced to 40 µAU hour The operating conditions are Sample wavelength 520 nm Sample bandwidth 10 nm Reference bandwidth 50 nm active reference mode only Flowing water at 1 0 mL min 10 35 MPa 1500 psi Figure 3 5 Effect of Reference Wavelength on Baseline Drift Reference Wavelength Mode Off Baseline Drift 120 µAU hour mAU min mi...

Page 48: ...en a reference wavelength active mode is selected When the reference wavelength is off the reference bandwidth is the same as the sample bandwidth Select a reference bandwidth in an area of the spectrum where the sample does not absorb The reference bandwidth should be narrow enough not to interfere with nearby compounds A wider bandwidth will reduce baseline noise but may increase the chance that...

Page 49: ...e Bandwidth Figure 3 6 shows the spectrum of caffeine The operating conditions are Sample wavelength 272 nm Sample bandwidth 5 nm Reference wavelength 325 nm Reference bandwidth 51 nm These settings calculate the absorbance by the following equation Figure 3 6 Caffeine Spectrum AU log avg IK 300 to 350 avg IK 210 to 274 offset at autozero ...

Page 50: ... more data points that are recorded and in general the more precise the analytical results However because collecting more data points requires more storage capacity the step setting sometimes represents a compromise between the amount of information collected and the file size The user does not need to select a step setting PeakNet 6 or Chromeleon automatically selects the step value that is the ...

Page 51: ...ise time and the average of the data points between steps If you select a larger step size when the average parameter is off the selected rise time is valid but some data points will be skipped Average The average parameter operates in conjunction with the step parameter see Step When average is On PeakNet 6 or Chromeleon averages the data points between step intervals reports that value and noise...

Page 52: ...an result in flat baselines or truncated peaks if this occurs increase the NegativeAbsorptionLevel setting to shift the detection level This is especially helpful when running a gradient application in which the absorbance decreases more than several hundred mAU For example in Figure 3 7 the NegativeAbsorptionLevel setting is 100 initially and the baseline is flat when the gradient is 50 The basel...

Page 53: ... run autozero and then check the intensity of the deuterium lamp Press F8 to display the Commands dialog box select UV and select LampIntensity The reading should be above 10 million counts if it is not select the UV_Calibration Intensity command to calibrate the lamp After calibration check the lamp intensity again If the reading is still too low clean the flow cell see Section 5 2 or replace the...

Page 54: ...og output channels whenever the detector power is on Use a chart recorder or other voltage measuring device to monitor the channels When the PDA 100 power is first turned on the analog output settings are at the factory defaults see the table below These factory default settings are also in effect Rise time 2 0 seconds Lamp status The deuterium and tungsten lamps are on Stand Alone Operation The t...

Page 55: ...itting 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 Withou...

Page 56: ...r tungsten lamp respectively Approximately every 6 months check the intensity of the deuterium lamp as follows Press F8 in PeakNet 6 or Chromeleon to display the Commands dialog box select UV to display UV related commands and select LampIntensity The reading should be above 10 million counts if it is not select the UV_Calibration Intensity command to calibrate the lamp After calibration check the...

Page 57: ...e software Audit Trail for an error message Deuterium LED is flashing The lamp did not power on properly Check the software Audit Trail for an error message If necessary replace the lamp see Section 5 7 If the LED flashes again there may be a bad connection between the lamp power supply and the lamp Contact Dionex Technical Support for assistance Tungsten LED is flashing The lamp did not power on ...

Page 58: ...ower on properly Press F8 in the software to display the Commands dialog box select UV to display UV related commands and check that UVLampPowerOnSetting and VisLampPowerOnSetting are Off If the LED continues flashing replace the lamp s See Section 5 7 or Section 5 8 for replacement instructions for the deuterium lamp or tungsten lamp respectively PDA 100 not detected on the DX LAN When the host c...

Page 59: ...ng mobile phase strength or composition The lamps usually require 20 to 30 minutes to stabilize For sensitive applications work or for detector validation allow at least 2 hours for the lamps to stabilize After installing a new lamp allow from 8 to 24 hours for the lamp to stabilize After changing mobile phases allow 20 to 30 column volumes for the system to stabilize If the noise is synchronized ...

Page 60: ...a visible wavelength is selected make sure the tungsten lamp is on Deuterium lamp is dimming The light output of the deuterium lamp decreases over time The lower light output may increase noise above an acceptable level especially after the lamp has been in service for more than 1000 hours If this occurs replace the lamp see Section 5 7 Tungsten lamp needs replacement Install a new tungsten lamp s...

Page 61: ... 1 Flow cell installed incorrectly Be sure the cell is inserted straight into the optical bench and is fully seated see Section B 4 2 Inappropriate rise time In general the rise time should be approximately 25 of the peak width at half height of the narrowest peak of interest See Section 3 4 for more information Detector exposed to high vibration Optical detectors are sensitive to vibrations Make ...

Page 62: ...t panel are in place optical components are sensitive to temperature and light Flow cell heat exchanger not in place Check that the flow cell inlet tubing is threaded through the tubing guide on the lamp cover and secured in place with the tubing bracket see Figure 5 1 Lamp not stabilized The lamps usually require 20 to 30 minutes to stabilize For sensitive applications work or for detector valida...

Page 63: ...ium lamp or tungsten lamp respectively The average lamp lifetime is 1000 hours although lamps often last longer with only minimal deterioration in performance 4 6 Deuterium Lamp Intensity Count Too Low If the deuterium lamp intensity reading is low see Section 3 6 follow these steps to resolve the problem Light signal is not reaching the data processor reading is 1000 counts Make sure that at leas...

Page 64: ...rt for assistance Blockage in cell Flush the cell with eluent 4 7 Wavelength Calibration Fails Flow cell contains air bubble or old mobile phase Flush mobile phase through the cell Cell not clear or mobile phase has high background absorbance Clean the cell as instructed in Section 5 2 If the detector fails the wavelength calibration again replace the flow cell windows see Section 5 5 Deuterium la...

Page 65: ...f solvent sits in the cell for an extended period it decreases the intensity of the light passing through the cell To ensure reliable data maintain a constant flow through the cell Flushing the cell with deionized water or methanol each time the detector is powered up is helpful Lamp is dimming Check the lamps as follows In PeakNet 6 or Chromeleon press F8 to display the Commands dialog box and se...

Page 66: ... DX LAN cable P N 960281 must be connected between the Ethernet hub P N 056909 and the DX LAN connector on the host computer s internal DX LAN interface card 4 10 No Spectra Collected Spectral range was not programmed Select a spectral range in the PGM file or control panel Detector and PGM file or control panel connected to different timebases Add the PDA 100 to the same timebase as the PGM file ...

Page 67: ...e bandwidth should not overlap the sample bandwidth 4 12 Peaks Too Large or Small Analog output related problem Check the recorder and integrator input voltage The PDA 100 provides a 1 volt full scale output Verify that the selected output range AU full scale is appropriate System level problem Verify that the sample volume or concentration is appropriate Verify that the rise time and data collect...

Page 68: ...ollow when selecting the sample wavelength refer to Section 3 4 Incorrect reference wavelength selected Select a different reference wavelength For guidelines to follow when selecting the reference wavelength refer to Section 3 4 Sample bandwidth too wide Select a bandwidth that provides the resolution required to achieve the desired sensitivity Narrow spectra peaks require narrow bandwidths A wid...

Page 69: ...ent and or clean the cell as instructed in see Section 5 2 Reinstall the cell in the optical bench and autozero the detector again to verify that the problem has been resolved If the error message appears again contact Dionex Technical Support for assistance If you see a weak light or no light at all shining onto the business card the lamp intensity is too low Check that the flange of the new lamp...

Page 70: ...udit Trail folder and the file for that date 4 15 2 Software Diagnostics and Calibration PeakNet 6 and Chromeleon contain comprehensive diagnostics for the PDA 100 This section briefly describes some of these diagnostics for a full description refer to the software Help or user s manual Lamp age Indicates the total number of hours that each lamp has been turned on in its lifetime To reset the lamp...

Page 71: ...on are stored in the calibration log and can be retrieved at any time To calibrate the wavelength a Press F8 to display the Commands dialog box b Select UV to display UV related commands c Select UV_Calibration and then WavelengthCal d Click the Execute button e When the calibration procedure is complete select the WavelengthCalResult command or click the Wavelength button on the PDA 100 Wellness ...

Page 72: ...PDA 100 Photodiode Array Detector 4 16 Doc 031644 02 9 03 ...

Page 73: ...eplaced dispose of the used battery according to local regulations Before replacing any parts review the troubleshooting information in Chapter 4 to isolate the cause of the problem 5 1 Liquid Leaks The PDA 100 is plumbed with the components listed below For tightening requirements refer to Installation of Dionex Ferrule Fittings Substituting non Dionex parts may impair the performance of the PDA ...

Page 74: ...g a syringe flush the cell with a succession of deionized water acetone and 3 M HNO3 4 Flush the cell with deionized water for 20 to 30 minutes at 1 0 mL min 5 Reconnect the cell liquid lines 5 3 Removing Trapped Air from the Flow Cell Trapped air bubbles in the flow cell may cause pulsations of the baseline or random noise and low readings Flush the cell with methanol for 20 minutes If this does ...

Page 75: ...nect the tubing connected to the flow cell inlet and outlet see Figure 5 1 3 Remove the flow cell cover from the inside front panel 4 Remove the tubing bracket from the lamp cover 5 Remove the flow cell inlet tubing from the tubing guide in the lamp cover 6 Squeeze the handle of the flow cell and pull it out of the optical bench Figure 5 1 Removing the Flow Cell Flow Cell Cover Lamp Cover Lamp Wir...

Page 76: ...placement kit P N 060498 contains all of the parts required for this procedure The kit is optional and must be ordered separately from the PDA 100 1 Remove the flow cell from the optical bench see Section 5 4 and place it on a clean work surface 2 Put on a pair of latex gloves 3 Using the windows replacement tool P N 060497 remove one of the window nuts from the flow cell see Figure 5 2 It does no...

Page 77: ...w cell if a colored substance stains the cell interior and cleaning the cell see Section 5 2 does not remove the stain or if excessive backpressure cracks the silica windows and you do not want to replace them see Section 5 5 1 Remove the flow cell from the optical bench see Section 5 4 2 Squeeze the handle of the new flow cell PEEK P N 056346 stainless steel P N 056126 and insert it straight into...

Page 78: ... see Figure 5 3 and pull the lamp out of the optical bench NOTE The screws are captive in the lamp base and do not need to be removed 10 Inspect the new deuterium lamp P N 939016T for fingerprints and dust If necessary clean the lamp with isopropyl alcohol IPA 11 Line up the flange of the new lamp with the two locating pins and three threaded holes in the optical bench see Figure 5 3 When the flan...

Page 79: ...ce the lamp cover 15 Thread the flow cell inlet tubing through the tubing guide on the lamp cover and reinstall the tubing bracket 16 Replace the flow cell cover and reconnect the inlet and outlet tubing 17 Replace the detector front panel 18 Turn on the detector power 19 Start the PeakNet 6 or Chromeleon server To ensure proper performance the lamp must be fully seated Do not pinch the UV lamp co...

Page 80: ...g box b Select UV to display UV related commands c Select UVLampAge d Reset the lamp age to zero e Click the Execute button NOTE It is normal for the baseline to drift for several hours after a new deuterium lamp is installed 21 Run the wavelength calibration and verification for the new lamp from the Wellness panel see Section 4 15 2 ...

Page 81: ... the side wall see Figure 5 3 9 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 10 Inspect the new tungsten lamp P N 056123T for fingerprints and dust If necessary clean the lamp with isopropyl alcohol IPA The lamp housing and base may be hot to the touch ...

Page 82: ...ide on the lamp cover and reinstall the tubing bracket 15 Replace the flow cell cover and reconnect the inlet and outlet tubing 16 Replace the detector front panel 17 Turn on the detector power 18 Start the PeakNet 6 or Chromeleon server 19 Reset the lamp lifetime as follows a Press F8 to display the Commands dialog box b Select UV to display UV related commands c Select VisLampAge d Reset the lam...

Page 83: ...e it The fuse holder pops out slightly when the lock is released Repeat for the other lock HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the PDA 100 HAUTE TENSION Débranchez le cordon d alimentation principal de sa source et du panneau arrière du PDA 100 HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der Rückseite des PD...

Page 84: ...ew 4 0 amp fast blow IEC 127 fuses P N 954763 Dionex recommends always replacing both fuses 5 Reinsert the fuse holder into the compartment The fuse holder is keyed to fit only in the correct orientation Apply pressure evenly against the holder until the locks are engaged When correctly installed the fuse holder is flush against the panel 6 Reconnect the power cord and turn on the power ...

Page 85: ...ING setting during routine operation 56 db at A WEIGHTING setting at power up Operating Temperature 4 ºC to 40 ºC 40 ºF to 104 ºF Operating Humidity 5 to 95 relative humidity noncondensing Main Power 85 Vac to 264 Vac 47 63 Hz The input power is 162 W maximum the output power is 130 W maximum The maximum input current is 4 amps The auto sensing power supply requires no voltage or frequency adjustm...

Page 86: ...xel Resolution 0 7 nm Wavelength Accuracy 1 nm Noise 10 µAU with 2 second rise time 254 nm 4 nm bandwidth and flowing deionized water 15 µAU with 2 second rise time 520 nm 10 nm bandwidth and flowing deionized water Drift 500 µAU hour after warm up Linearity 2 AU Analog Outputs Four built in analog outputs Voltage Out 1 V output Analog Output Range 0 0005 0 001 0 01 0 1 0 5 1 0 2 0 or 3 0 AU full ...

Page 87: ...m Operating Pressure PEEK cell 2 MPa 300 psi Stainless steel cell 3 MPa 500 psi Chemical Compatibility Do not use bases stronger than 0 1 M they will etch the silica windows of the flow cells Do not use normal phase or chlorinated solvents with the PEEK flow cell they will damage the cell Do not use high pH salts with the stainless steel flow cell they will cause corrosion contamination and metal ...

Page 88: ...PDA 100 Photodiode Array Detector A 4 Doc 031644 02 9 03 ...

Page 89: ... unless the front panel flow cell cover and lamp cover are in place Optical detectors are sensitive to vibrations Make sure the PDA 100 installation site is vibration free B 2 Unpacking Carefully remove the PDA 100 from the shipping container Do not turn on the PDA 100 unless it is at room temperature 10 ºC to 40 ºC 50 ºF to 104 ºF If the detector is moved from a cold environment to a warm environ...

Page 90: ...t is located near the PDA 100 and is easily accessible Operation at AC input levels outside of the specified operating voltage range may damage the PDA 100 DANGER D ÉLECTROCUTION Pour éviter toute électrocution il faut utiliser une prise de courant avec prise de terre Ne l utilisez pas et ne le branchez pas au secteur C A sans utiliser de branchement mis à la terre Le cordon d alimentation princip...

Page 91: ...NG H3 15A 250V XXXXXXXX TUV MODEL PDA 100 INPUT 100 240V 50 60Hz 1 5A SERIAL NUMBER 035779 05 Made in U S A Dionex Corporation Sunnyvale California 94086 An alternative license is available on reasonable terms to practice any of the foregoing methods of use which can be praticed without infringing patented apparatus or products Apparatus and products manufactured and sold by Dionex Corporation und...

Page 92: ...a flow rate of 1 0 mL min 2 meters for 0 5 mL min and so on c Install a ferrule fitting and 10 32 bolt on each end of the tubing d Install the backpressure line after the cell outlet Use a union P N 042627 to connect the backpressure line to the waste line 4 The cell connections exit the detector through slots in the front panel Thread the cell outlet tubing through the slot near the bottom of the...

Page 93: ...0 provides four analog outputs controlled by absorbance wavelengths 1 through 4 in PeakNet 6 or Chromeleon software They provide a 1 volt output maximum The software controls the full scale absorbance output and offset within the 0 to 1 volt range Connect a recorder or an integrator to the ANALOG OUT connector on the PDA 100 rear panel see Figure B 1 The drain tube must remain below the drain port...

Page 94: ...mA at 5V or higher it may damage the Data Processing card SHOCK AND FIRE HAZARD Inputs and outputs are not rated for connection to an AC power main DO NOT CONNECT TO 100 115 220 230 OR 240 VAC POWER SOURCES FIRE OR ELECTROCUTION MAY RESULT DANGER D ÉLECTROCUTION ET D INCENDIE Le module d alimentation électrique fonctionne aux potentiels du secteur Faites effectuer toutes les réparations par un per...

Page 95: ...ent 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 Remote inject 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 i...

Page 96: ...10BASE T cable P N 960281 from a 10BASE T port on the hub to the 10BASE T port on the host computer s internal DX LAN card If the connection is via port 8 on the hub set the Normal Uplink push button to Normal NOTE Installation instructions for the host computer s internal DX LAN card are in Installing the Dionex PeakNet 6 System Document No 031631 Cascading Hubs Cascading or connecting hubs toget...

Page 97: ...A 100 with PEEK Flow Cell 056346 PEEK Flow Cell with heat exchangers 1 060037 PEEK Flow Cell Outlet Tubing Assembly 1 043276 Ferrule 1 043275 Nut 1 060498 Flow Cell Windows Replacement Kit 1 PDA 100 with Stainless Steel Flow Cell 056126 Stainless Steel Flow Cell with heat exchangers 1 060038 Stainless Steel Flow Cell Outlet Tubing Assembly 1 055902 Union Fitting 1 010262 Ferrule 1 010261 Nut 1 060...

Page 98: ...PDA 100 Photodiode Array Detector C 2 Doc 031644 02 9 03 ...

Page 99: ...cting 3 25 B Backpressure B 4 Slow increase 3 29 Sudden increase 3 29 Backpressure line 4 4 B 4 Bandwidth 3 8 Setting is too narrow 4 5 Baseline drift 3 15 Reducing 3 20 Baseline noise 3 15 5 2 Causes 5 2 Reducing 3 16 3 19 3 20 3 22 4 12 Relationship to rise time 3 16 Baseline offset 2 9 Bolts 10 32 Part number B 4 Buffers 3 2 Bunch width 3 8 3 15 Guidelines for selecting 3 24 C Cable DX LAN Inst...

Page 100: ...uch disk space 3 17 Data points 3 17 3 24 Minimum number per peak 3 17 Data Processing card 2 9 Analog output connectors 2 9 Lithium battery disposal 5 1 Deuterium lamp 2 4 2 5 Calibration 4 8 Lamp does not light 4 7 Maintenance 3 30 Output waning 4 4 Part number 5 6 Power supply 2 8 Replacing 5 6 See also Lamps Time in use 5 8 Time to stabilize 3 4 4 3 4 6 Deuterium LED 2 1 Flashing 2 1 4 2 4 7 D...

Page 101: ...ation 2 3 Installation Instructions B 3 B 5 B 7 Site requirements A 1 B 1 Integrator 4 11 B 5 Isocratic analyses Reference wavelength selection 3 20 4 7 L Lamp power supply 2 8 Lamps 1 1 Calibration 4 8 Deuterium LED flashing 2 1 Failure 2 1 2 2 Installation procedures 5 6 5 9 Maintenance 3 30 See also Deuterium lamp See also Tungsten lamp Tungsten LED flashing 2 2 Leak alarm 2 3 Leak sensor 2 3 L...

Page 102: ...wer cord B 2 Power supply 2 7 A 1 B 2 Power switch B 2 Safety standards 1 6 Ship Kit B 1 B 4 Shutdown procedure 3 29 Spare parts C 1 Tubing connections 5 1 Unpacking instructions B 1 Warranty 5 1 Weight A 1 Peak height 3 16 3 19 Peak identification 1 2 1 3 3 18 Peak purity 1 2 1 3 3 5 3 18 Peak resolution 3 15 PeakNet 6 software 1 1 3D option 1 2 3 5 Control of PDA 100 3 5 3 8 3 9 Leak alarm 2 3 S...

Page 103: ... 3 20 3 22 4 6 Definition 3 20 Guidelines for selecting 3 20 Inappropriate setting 4 4 Relay control 2 12 Installation B 6 Pin assignments B 7 Replacing parts 5 1 Use of non Dionex parts 5 1 Retention time 3 1 Rise time 2 9 3 15 Correlation with data collection rate 3 17 Definition 3 16 Effect on baseline noise 3 16 Guidelines for selecting 3 16 3 17 Inappropriate setting 4 5 Run LED 2 1 Flashing ...

Page 104: ...ication problem 4 2 4 10 Elution time is slow 4 3 Lamp does not light 4 7 PDA 100 does not respond 4 2 4 3 Peak shape is poor 4 12 Peak size is wrong 4 11 Spectra not collected 4 10 Spectral resolution is poor 4 10 Wavelength calibration fails 4 8 Wavelength verification fails 4 9 TTL control 2 12 Installation B 6 Pin assignments B 7 Tubing connections 3 2 5 1 Maintenance 3 29 Tungsten lamp 2 4 2 ...

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Dionex PDA-100, Operator'S Manual

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