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4 

Xcalibur Diagnostics for the PDA Detector

Calibrating the PDA Detector from the Xcalibur Data System

Thermo Scientific

Accela PDA Detector Hardware Manual

55

Figure 48. 

Page 8 of the Wavelength Calibration wizard 

11. Check that the delta values are within ±1 nm, and then do one of the following: 

• If the Delta values are acceptable, proceed to 

step 12

.

• If the delta values are not within the range of ±1 nm, do not export the results, and 

proceed to 

step 13

. Complete the calibration procedure, and then repeat the 

wavelength calibration. If, after applying a second calibration, the Delta values are 
still not within the range of ±1 nm, call your Thermo Fisher Scientific service 
representative for assistance.

12. (Optional) Print a report of the calibration results:

a. Click 

Export Results

 to print the results to a file. 

The Save As dialog box appears (see 

Figure 49

).

Содержание Accela PDA

Страница 1: ...Accela PDA Detector 80 hertz data rate Hardware Manual 60257 97080 Revision A August 2009...

Страница 2: ...change without notice All technical information in this document is for reference purposes only System configurations and specifications in this document supersede all previous information received by...

Страница 3: ...compliance with EMC and safety standards replacement parts and additional components options and peripherals must be ordered from Thermo Fisher Scientific or one of its authorized representatives Acce...

Страница 4: ...by the instrument Notice on the Susceptibility to Electromagnetic Transmissions Your instrument is designed to work in a controlled electromagnetic environment Do not use radio frequency transmitters...

Страница 5: ...Directives and the recyclers in your country WEEE Konformit t Dieses Produkt muss die EU Waste Electrical Electronic Equipment WEEE Richtlinie 2002 96 EC erf llen Das Produkt ist durch folgendes Symb...

Страница 6: ...ieurs compagnies de recyclage dans chaque tat membre de l union europ enne et ce produit devrait tre collect ou recycl par celles ci Davantage d informations sur la conformit de Thermo Fisher Scientif...

Страница 7: ...si raffreddino prima di effetturare l intervento di manutenzione Fire Use care when operating the system in the presence of flammable gases Feuer Beachten Sie die einschl gigen VorsichtsmaBnahmen wen...

Страница 8: ...and proper procedures to dispose waste oil Heat Before servicing the instrument allow any heated components to cool Fire Use care when operating the system in the presence of flammable gases Eye Haza...

Страница 9: ...allation 9 Installation Checklist 10 Unpacking and Inspecting the Instrument 11 Making Initial Instrument Preparations 11 Making the Back Panel Connections 12 Connecting the Ethernet Cable 12 Connecti...

Страница 10: ...Event Log 57 Checking the Firmware Version 59 Chapter 5 ChromQuest Diagnostics for the PDA Detector 61 Accessing the Direct Controls for the Accela PDA Detector 62 Controlling the Lamps from the Chro...

Страница 11: ...al xi Replacing the Lamps 89 Replacing the Fuses 95 Chapter 7 Troubleshooting 97 Detector Related Problems 97 Log Entries 100 Critical Failure Messages 100 Warning Messages 101 Information Messages 10...

Страница 12: ......

Страница 13: ...ting Connected Guide Accela Getting Started with Xcalibur Guide ChromQuest User Guide for the Accela UHPLC The Thermo Scientific data system that you use to control the PDA detector has a built in Hel...

Страница 14: ...the waste bottle Read the safety labels inside the lamp compartment before you remove the lamp cover CAUTION Highlights electrical shock hazards CAUTION Highlights UV radiation hazards CAUTION Highli...

Страница 15: ...iew of the exposed optical fibers at the inlet end of the LightPipe flowcell Drainage Connections Before you start the solvent flow from the pump make sure that the solvent flow from the outlet end of...

Страница 16: ...old to a sealed waste bottle Figure 2 on page xvi Figure 2 Drain connected to waste bottle Power Communication Run Degas ACCELA Pump Power Communication Run Temperature ACCELA Autosampler Power Commun...

Страница 17: ...lug the power cord from line power After you pull the PDA detector s chassis partially out of the housing you can see the heat UV radiation and electrical shock caution labels inside the lamp compartm...

Страница 18: ...romatogram of a typical sample and standard mixture well documented with system conditions for future reference Careful comparison of retention times peak shapes peak sensitivity and baseline noise ca...

Страница 19: ...ration Remember that some solvents can corrode stainless steel Solvent Disposal Make sure you have a solvent waste container or other kind of drain system available at or below the benchtop level Most...

Страница 20: ...o to mssupport thermo com and click Customer Manuals in the left margin of the window Y To suggest changes to documentation or to Help To provide us with comments about this document click the link be...

Страница 21: ...roduction The Accela PDA Detector is a member of the Accela family of ultra high performance LC instruments see Figure 1 Figure 1 Accela PDA Detector Contents Functional Description LightPipe Flowcell...

Страница 22: ...ungsten halogen lamp for detection in the visible wavelength range 360 to 800 nm The light output from the two lamps overlaps in the 300 to 500 nm range You can increase or decrease the light intensit...

Страница 23: ...cally interpolates diode intervals to arrive at integer wavelengths The photodiode array is mounted on the Array Acquisition PCB which also contains all the analog detection circuitry The PDA detector...

Страница 24: ...install the LightPipe flowcell Replace the protective end caps for storage if you remove the LightPipe flowcell from the detector Figure 4 End of the LightPipe flowcell Figure 5 LightPipe flowcell wi...

Страница 25: ...ling time both increase the detector noise level These topics provide guidance on minimizing detector noise and maximizing the useful lamp lifetime Controlling the Amount of Light that Reaches the Dio...

Страница 26: ...hysical limit sooner at the higher diode array scan rates The useful lifetime of the lamp depends on the acceptable noise level for your application At the 20 Hz diode array scan rate you can compensa...

Страница 27: ...Communication to the data system PC has been established Amber There is no communication with the data system Run Green The detector is ready for a run Flashing green A run is in progress and the det...

Страница 28: ...can rate 20 40 or 80 Hz user selectable Rise time 0 0 0 02 0 05 0 1 0 2 0 5 1 2 5 or 10 s user selectable Cell dimensions 10 mm LightPipe flowcell or 50 mm LightPipe flowcell Cell pressure rating 1000...

Страница 29: ...that you can use as a quick reference for conducting a successful installation Make a copy of the checklist fill it out when the installation is complete and include it in your maintenance records Con...

Страница 30: ...rst time See page 24 U Install software and connect remote communication outputs as required See page 21 U Configure the Accela PDA Detector for control from your chromatography data system See Chapte...

Страница 31: ...ing contact your Thermo Fisher Scientific representative immediately The part numbers of the accessory kit items are listed in Table 11 on page 104 Making Initial Instrument Preparations Place the PDA...

Страница 32: ...ernet switch to the data system computer using the supplied CAT5 7 ft long shielded Ethernet cable with ferrite clamp Connecting the System Interconnect Cable The system interconnect cable coordinates...

Страница 33: ...uide Figure 8 Seven connector version of the system interconnect cable Figure 9 Back panel of Accela PDA Detector DETECTOR DETECTOR DETECTOR PUMP PUMP A S M S Autosampler connector 1 2 3 4 5 6 7 8 9 0...

Страница 34: ...rounded at just one end The ends 1 4 in of the analog signal wires are stripped and soldered to allow electrical contact and to prevent fraying On the detector s back panel there are two analog output...

Страница 35: ...value of 01 The range of values for the unit ID is 01 to 99 The value of 00 is reserved for special service functions The unit ID must correspond with the stack ID specified in the Instrument Configur...

Страница 36: ...hromQuest data system If you use a TTL signal to trigger the external device connect the PDA EVENT terminal pin 8 to the positive pin on the external device input and connect one of the PDA GND termin...

Страница 37: ...rs for these items are listed in Table 6 on page 103 Y To install the LightPipe flowcell 1 Open the front doors of the detector 2 Unscrew the captive screw that secures the LightPipe flowcell access c...

Страница 38: ...e LC column outlet 6 Connect the outlet port of the LightPipe flowcell If you are not connecting to an MS detector use a PEEK fitting to connect the blue 0 010 in ID outlet tubing to the LightPipe flo...

Страница 39: ...tlet fitting on the top right side see Figure 16 Figure 15 Location of the inlet and outlet tubing for the 10 mm LightPipe flowcell 8 Replace the LightPipe flowcell retaining block 9 Reinstall and han...

Страница 40: ...ll 10 Replace the flowcell access cover ensuring that the inlet and outlet tubing pass through the slots see Figure 13 on page 17 without being pinched Tighten the captive screw to secure the flowcell...

Страница 41: ...polarity settings active high or active low of these outputs must match those of the inputs of connecting equipment Setting the Remote Output Polarities from the Xcalibur Data System Y To set the pola...

Страница 42: ...the Accela PDA Direct Control dialog box Xcalibur data system 8 In the Analog Outputs area of the Configuration page check the current settings of the outputs 9 Change the settings to match the connec...

Страница 43: ...ady done so 2 Add the Accela PDA Detector to the instrument configuration see ChromQuest Data System Instrument Configuration on page 30 3 Open the Instrument window 4 Choose Control Instrument Status...

Страница 44: ...on 4 Check the fuse size see Replacing the Fuses on page 95 You can operate the PDA detector at 100 115V or 230V However you must ensure that the appropriate fuses are installed see Figure 19 and Tabl...

Страница 45: ...ith use monitor the integrated light intensity of the diodes as part of a routine maintenance program and adjust the attenuators when you notice an increase in baseline noise Because the diode array s...

Страница 46: ...ific For information on calibrating your PDA detector and adjusting the light throughput to the diode array see the chapter for your data system For the ChromQuest data system see Chapter 5 ChromQuest...

Страница 47: ...e array scan rate You set the unit ID is set by adjusting the two rotary switches on the back panel of the detector The switches are set to 01 at the factory see Figure 21 Do not adjust the switches u...

Страница 48: ...To configure your instrument in Thermo Foundation 1 Open the Instrument Configuration application For Xcalibur 2 1 or higher from the computer desktop choose Start All Programs Thermo Foundation 1 0...

Страница 49: ...rray Scan Rate area select the appropriate diode array scan rate for your application The appropriate diode array scan rate depends on the baseline width Wb of your application s chromatographic peaks...

Страница 50: ...og box appears Figure 24 Go to step 5 For ChromQuest go to step 2 2 If you have not already done so create an instrument for your Accela LC stack a Double click the ChromQuest icon on the Windows XP d...

Страница 51: ...ck OK in the message dialog box that appears 7 Click Configure The Accela dialog box appears 8 In the Available modules pane double click the Detector button The Analog icon appears in the Configured...

Страница 52: ...rate for your application The appropriate diode array scan rate depends on the baseline width Wb of your application s chromatographic peaks 10 Click OK to accept the settings and close the Accela PDA...

Страница 53: ...rformance can change With use the deuterium lamp produces less and less light so that the system performance changes as the lamp s lifetime hours increase To verify the proper operation of the PDA det...

Страница 54: ...s perform diagnostics and calibrate the PDA detector Y To open the Accela PDA Direct Control dialog box 1 On the Thermo Xcalibur Roadmap view click the Instrument Setup button The Instrument Setup vie...

Страница 55: ...tors as described in Adjusting the Light Throughput with the Xcalibur Data System on page 42 does not help replace the lamps The detector keeps track of the number of hours each lamp has been operatin...

Страница 56: ...associated lamp The stored total run time for the associated lamp resets to zero and the Last Lifetime Reset readback is updated to the current date and time Setting the Startup Time for the Lamps Y T...

Страница 57: ...ould start the lamps at box Then use the keyboard arrow keys the number keys or both to change the time 5 Click OK to apply the new lamp startup time Use the Programmed Start option to pre warm the la...

Страница 58: ...Make sure that the lamps are on and equilibrated a Click the Configuration tab The Configuration page appears see Figure 28 on page 35 b Check the status and usage of each lamp c If they are not alrea...

Страница 59: ...the Diodes Intensity option b To make the scan parameters available select the Collect Spectral Data check box The default settings for the Diode Intensity option appear Use these settings to view th...

Страница 60: ...em saves the file with an spda file extension Viewing an Intensity Scan Y To view an intensity scan 1 From the menu bar of the Accela PDA view in the Instrument Setup window choose Accela PDA Direct C...

Страница 61: ...um plot 5 To start the data stream click Start Data see Figure 32 The Spectrum and Channels plots begin to update and the Start Data button changes to the Snapshot button 6 Press ALT PRINT SCREEN to s...

Страница 62: ...nfigured diode array scan rate see Thermo Foundation Instrument Configuration on page 28 Y To adjust the attenuators while viewing the light intensities 1 Prepare the PDA detector to monitor an intens...

Страница 63: ...80 This spike is an emission line of the deuterium lamp 4 Adjust the left attenuator tab UV attenuation to achieve a Channel A value as close as possible to 900000 intensity counts without saturating...

Страница 64: ...array calibration dark current after any of the following events occurs After 100 hours of use or monthly whichever comes first Whenever a significant temperature change occurs After you move the dete...

Страница 65: ...alibrate The preconditions page appears see Figure 34 Figure 34 Preconditions page 5 Read the preconditions and verify that they have been met If the preconditions have been met click Next to proceed...

Страница 66: ...or Hardware Manual Thermo Scientific Figure 35 Page 2 of the Dark Current Calibration wizard 7 When the calibration is complete click Next Page 3 of the Dark Current Calibration wizard appears see Fig...

Страница 67: ...name and then click Save After you save the file with a name of your choice you can view or print the contents of the file using any text editing program see Figure 37 Figure 37 Accela PDA dark curren...

Страница 68: ...Detector Hardware Manual Thermo Scientific 10 Click Finish The detector stores the calibration results The date and time of the calibration appears in the Dark Current Calibration area of the Calibra...

Страница 69: ...the photodiode array Use the automated wavelength calibration to determine wavelength accuracy and to correct for any misalignment Y To perform a wavelength calibration from the Xcalibur data system...

Страница 70: ...tion wizard see Figure 42 do the following a Select a peak set from the list The peak set should span the wavelengths you use under normal operating conditions Figure 42 shows the selection of the Hol...

Страница 71: ...Detector from the Xcalibur Data System Thermo Scientific Accela PDA Detector Hardware Manual 51 Figure 42 Page 2 of the Wavelength Calibration wizard with a list of calibration files b Click Next Pag...

Страница 72: ...Page 3 of the Wavelength Calibration wizard 5 Do the following a Observe the status screen that tells you the wavelength file is being downloaded see Figure 43 b When you see the message Click the Ne...

Страница 73: ...ration Wizard appears see Figure 45 Figure 45 Page 5 of the Wavelength Calibration wizard 8 Do the following a Observe the status screen see Figure 45 The diagnostics program waits for a few seconds f...

Страница 74: ...Page 6 of the Wavelength Calibration wizard 9 Rotate the wheel back to position 1 Open as instructed on page 6 of the Wavelength Calibration wizard see Figure 46 The Next button becomes active see Fi...

Страница 75: ...able proceed to step 12 If the delta values are not within the range of 1 nm do not export the results and proceed to step 13 Complete the calibration procedure and then repeat the wavelength calibrat...

Страница 76: ...System 56 Accela PDA Detector Hardware Manual Thermo Scientific Figure 49 Save As dialog box b In the File name box type a name and then click Save You can view or print the calibration results using...

Страница 77: ...to a dedicated area in the memory of the detector These messages are created as part of the normal operation of the detector and can be helpful when you are attempting to troubleshoot communications...

Страница 78: ...a To retrieve and display information from the detector click Request Log Figure 52 on page 58 shows a sample log Review the log For a list of some common error messages that might appear in the log...

Страница 79: ...sher Scientific Service Representative about the availability of new firmware Y To check the firmware version 1 Open the Accela PDA Direct Control dialog box see Opening the Accela PDA Direct Control...

Страница 80: ......

Страница 81: ...ium lamp produces less and less light so the system performance changes as the lamp s remaining lifetime hours decrease For information on configuring your Accela PDA Detector see ChromQuest Data Syst...

Страница 82: ...Programs Chromatography ChromQuest The Main Menu window appears 2 Double click the instrument icon that represents your LC stack The Instrument window appears 3 In the menu bar choose Control Instrum...

Страница 83: ...ge 5 As lamps age they emit less light which results in increased baseline noise If the noise level of your detector signal is unacceptable and cleaning the LightPipe flowcell does not help use the di...

Страница 84: ...The Status readback displays Starting during the 10 second ignition period and then it changes to On If there is a problem with the lamp the Status readback displays Failed In the W Lamp area click On...

Страница 85: ...monitor lamp performance from the ChromQuest data system 1 Open the Instrument window for your LC system a From the computer desktop choose Start All Programs Chromatography ChromQuest The Main Menu w...

Страница 86: ...rmo Scientific Figure 56 Control page with the default Spectrum settings 8 In the Discrete Channels area use the default settings or specify the diodes that you want to monitor 9 Click Load To Detecto...

Страница 87: ...k On in the Status area but before you click Start 12 On the right side of the page in the Status area click On 13 In the Data area click Start to refresh the display 14 Save a printout or an electron...

Страница 88: ...trum window and right click 2 From the shortcut menu choose Utilities Print Taking a Snapshot Use the snapshot option to create a Microsoft Excel comma separated values CSV file that contains informat...

Страница 89: ...tensities in the specified operating ranges To adjust the light throughput from the lamps follow these procedures 1 Setting Up the Spectral and Discrete Channel Displays 2 Adjusting the Attenuators Ti...

Страница 90: ...1 Step 1 d Click Load To Detector 4 Determine the diodes of maximum output for the lamps as follows From the spectrum displayed determine and record the pixel of maximum intensity within the 10 to 40...

Страница 91: ...e Channel Displays on page 70 2 Click the Display tab The Display page appears 3 As you view the discrete channel display see Figure 58 do the following Adjust the left attenuator tab UV attenuation t...

Страница 92: ...UV region Figure 60 shows a diode array that is saturated in both the UV and visible regions The configuration is set to a 20 Hz diode array scan rate and the attenuators are completely open Figure 60...

Страница 93: ...t saturated see Adjusting the Light Throughput with the ChromQuest Data System on page 69 Performing an Array Calibration from the ChromQuest Data System The Array calibration measures and corrects fo...

Страница 94: ...ibration tab The Calibration page appears 4 In the Array area click Execute A message box appears see Figure 61 Figure 61 Calibration preconditions dialog box 5 Make sure that the lamps are warmed up...

Страница 95: ...r is sharply jolted in shipping for example Such bumps and jars can slightly change the wavelength of light reaching the photodiode array The automated wavelength calibration determines the wavelength...

Страница 96: ...ropriate wavelength file should include the range of wavelengths that you use under normal operating conditions c Click Open The holmium oxide bands of the selected file appear in the Wavelength File...

Страница 97: ...lmium12 Wavelength Calibration File selected 4 In the Wavelength area click Execute A message box appears see Figure 65 Figure 65 Calibration preconditions 5 If all of the preconditions are met click...

Страница 98: ...andwidth filters and then displays a new message box see Figure 67 Figure 67 Calibration message prompting you to return the filter wheel to position 1 7 Move the filter wheel back to position 1 and t...

Страница 99: ...list of acceptable delta values 9 If your data system computer is connected to a printer click Print to print a hardcopy report To store the results click Export The date and time of the wavelength ca...

Страница 100: ...print out the log and clear it periodically The memory is protected by battery backup when the detector is turned off View print and clear the log weekly as part of your regular maintenance routine F...

Страница 101: ...ermo Fisher Scientific Service Representative about the availability of new firmware Y To check the firmware version in the ChromQuest data system 1 Open the Diagnostics dialog box see Accessing the D...

Страница 102: ......

Страница 103: ...egular basis If you have any questions on proper maintenance or would like to arrange for a preventive maintenance program contact your Thermo Fisher Scientific service representative For maintenance...

Страница 104: ...rrent calibration Calibrating the dark current increases the linearity of the detector at the high end of its operating range The dark current does not significantly affect absorbance values between 0...

Страница 105: ...l spiking erratic or drifting baselines low light intensity or increased backpressure This section contains the following procedures Removing the LightPipe Flowcell Cleaning the LightPipe Flowcell wit...

Страница 106: ...86 Accela PDA Detector Hardware Manual Thermo Scientific Figure 70 Accela PDA Detector with the front doors open Figure 71 Retaining block and retaining block knob Flowcell access cover Captive screw...

Страница 107: ...clean the LightPipe flowcell with an organic solvent 1 Remove the column from the chromatographic system to avoid column degradation Connect the inlet of the LightPipe flowcell directly to the chromat...

Страница 108: ...events possible leaks from harming the mechanical and electronic components of the detector 2 Ensure that the column is removed from the chromatographic system to avoid column degradation Connect the...

Страница 109: ...tungsten halogen lamp is relatively stable as the lamp ages The detector keeps track of the number of hours each lamp has been operating The deuterium lamp has a lifetime of approximately 1000 hours a...

Страница 110: ...mpartment to cool to room temperature 3 Turn the power switch at the front of the PDA detector to Off released position and disconnect the power cord from the back panel 4 If you did not turn off the...

Страница 111: ...hassis to the housing These screws are located on either side of the front panel see Figure 74 Figure 74 Four screws that secure the chassis to the housing 10 Slide the chassis out of the housing unti...

Страница 112: ...ch the lamp cover to make sure that it has cooled to room temperature and then carefully lift the lamp cover out of the detector IMPORTANT Do not try to remove the lamps from their mounting assemblies...

Страница 113: ...connector latch and then gently pull the connector free from the receptacle on the lamp compartment wall see Figure 76 b Loosen but do not remove the two Phillips head screws by turning them approxima...

Страница 114: ...atch and then gently pull the connector free from the receptacle on the lamp compartment wall see Figure 76 b Loosen and remove the single Phillips head screw that secures the lamp mounting block see...

Страница 115: ...nd unplug the detector from line power 2 Insert the tip of a narrow blade screwdriver into one of the two openings on the exterior surface of the power entry module and then apply leverage to gain acc...

Страница 116: ...r entry module door loosened 3 Open the door see Figure 80 Figure 80 Power entry module door opened 4 Take the loose fuse holder out of the power entry module see Figure 81 Figure 81 View of the fuse...

Страница 117: ...etector Related Problems Log Entries Table 5 Detector related problems Sheet 1 of 4 Symptom Cause Remedy Spikes on baseline Continuous gas bubbles in the LightPipe flowcell Degas the mobile phase Conn...

Страница 118: ...owcell or lamps Clean the dirty component Integrator input voltage does not match detector output voltage Verify that the integrator is connected to the appropriate Analog Output connections on the ba...

Страница 119: ...the rise time selection Poor connection at LightPipe flowcell inlet Check the end of the inlet tubing for a clean flat surface that is free of obstructions Detector does not power up Tripped circuit...

Страница 120: ...the PDA cannot perform its function properly If a chromatographic run is in progress when a critical failure occurs the data might be corrupted or lost and the run terminates Possible critical failure...

Страница 121: ...a null queue Error trying to receive from a null queue Socket failed to receive data Socket failed to send data Data in EEPROM was corrupted Failed to calibrate dark current Failed to calibrate wavel...

Страница 122: ......

Страница 123: ...iption 60053 98017 1 cm LightPipe flowcell with tubing and fittings 60053 98016 5 cm LightPipe flowcell with tubing and fittings 2522 0285 FingerTight 10 32 one piece PEEK fitting 803260 Inlet tubing...

Страница 124: ...on Table 10 Repair and service parts Part number Description 60262 61000R Assy CPU PCBA 60262 61200R Assy PCB lamp power supply board 00012 01 00023 Low Voltage Power Supply PCB 60257 63002 Cooling fa...

Страница 125: ...75 cleaning procedures external surfaces 85 LightPipe flowcell 85 compliance WEEE v configuration in ChromQuest 30 in Xcalibur 28 connections analog output 14 Ethernet 12 LightPipe flowcell 18 remote...

Страница 126: ...in ChromQuest 64 in Xcalibur 35 usage hours resetting in ChromQuest 64 in Xcalibur 36 useful lifetime 5 wavelength range 2 LEDs front panel 7 light intensity adjusting in ChromQuest 69 adjusting in X...

Страница 127: ...2 specifying in Xcalibur 29 status LEDs 7 storage temperature 8 T tools installation 11 lamp replacement 90 troubleshooting 97 tungsten halogen lamp See also lamps lifetime 89 U unit ID 15 UPS uninter...

Страница 128: ......

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