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Agilent Technologies 55B AA User Manual

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  • Page 1 Agilent 55B AA Spectrometer User’s Guide...
  • Page 2 DFAR 252.227-7014 (June understood and met. 1995), or as a “commercial item” as defined in FAR 2.101(a) or as “Restricted computer software” as defined in FAR 52.227-19 (June 1987) or any equivalent agency regulation or Agilent 55B AA Spectrometer User’s Guide...

  • Page 3: Table Of Contents

    Gas Hoses and Connections Ultraviolet Radiation Other Warning Symbols CE Compliance Electromagnetic Compatibility EN55011/CISPR11 ICES/NMB-001 Flame Operation Flammable Solvents Compressed Gases and Cylinders Acetylene Nitrous Oxide Burners Nebulizer Liquid Trap Heat Hazards Perchloric Acid Agilent 55B AA Spectrometer User’s Guide...
  • Page 4 Environmental Specifications Gas Supplies 3. Installation Instrument Overview Connections Power Moving Your Instrument Lamp Compartment Hollow Cathode Lamps Lamp Sample Compartment Nebulizer Spraychamber Burner Sample Compartment Front Panel Flame Shield 4. Interface Introduction Display Agilent 55B AA Spectrometer User’s Guide...
  • Page 5 Method Development Selecting the Language of the Interface Loading a Method Setting the Instrument Parameters Setting the Measurement Parameters Defining the Calibration Standards Saving/Deleting Methods Optimization Aligning Lamps Aligning the Burner Lighting the Flame Agilent 55B AA Spectrometer User’s Guide...
  • Page 6 Displaying the Calibration Graph Resloping the Calibration Sample Measurement Measuring Samples Manually Measuring Samples with SIPS Results Printing the Results Output to LIMS System Shutting Down the System 6. Maintenance Maintenance Schedule Daily Weekly Yearly Cleaning General Agilent 55B AA Spectrometer User’s Guide...
  • Page 7 Reassembling the Nebulizer Impact Bead Removing the Impact Bead Installing and Adjusting the Impact Bead Spraychamber Disassembling the Spraychamber Cleaning the Spraychamber Gas Supplies Lamp Fuses 7. Spare Parts Sample Introduction Other Covers/Doors Fuses Miscellaneous Agilent 55B AA Spectrometer User’s Guide...
  • Page 8 9320 No Peak: High BC Lamp Energy 9321 No Peak: Low HC Lamp Energy 9322 No Peak: High HC Lamp Energy 9323 Low Emission: No Peak 9324 High Emission: No Peak 9329 No Peak detected 9330 No Peak detected Agilent 55B AA Spectrometer User’s Guide...
  • Page 9 9921 Flame Out Detected 9922 Flame Shutdown: Gas type 9923 Flame Ignition Timeout 9934 Flame Shutdown: host offline 9937 Flame Pressure Relief Bung 9938 Liquid Trap Not Ready 9xxx GPIB Fault 9xxx Instrument Error 9xxx SpectrAA Error Agilent 55B AA Spectrometer User’s Guide...
  • Page 10 Contents This page is intentionally left blank. Agilent 55B AA Spectrometer User’s Guide...

  • Page 11: Safety Practices And Hazards

    Nebulizer Liquid Trap Heat Hazards Perchloric Acid Flashbacks Your Agilent 55B AA instrument and accessories have been carefully designed so that when used properly you have an accurate, fast, flexible and safe analytical system. Agilent 55B AA Spectrometer User’s Guide...

  • Page 12: Verifying Safe State

    Electrical Hazards The instrument and accessories contain electrical circuits, devices and components operating at dangerous voltages. Contact with these circuits, devices and components can cause death, serious injury, or painful electric shock. Agilent 55B AA Spectrometer User’s Guide...

  • Page 13: Heat, Vapors And Fumes

    Locate the system outlet such that the exhaust cannot re- enter the building through any door, window, air conditioning inlet, or other ventilator. Construct the system in accordance with local codes and regulations for ventilation. Agilent 55B AA Spectrometer User’s Guide...

  • Page 14: Compressed Gases And Cylinders

    Secure all cylinders to an immovable structure or a properly constructed cylinder stand. The area in which cylinders are stored must be adequately ventilated to prevent toxic or explosive accumulations. Move cylinders only on a properly constructed trolley. Agilent 55B AA Spectrometer User’s Guide...

  • Page 15: Gas Hoses And Connections

    Ensure that all gas connectors and hoses are correctly assembled. Arrange gas hoses so that they will not be damaged, stepped on, or have things dropped on them. Never use frayed or damaged hoses. Agilent 55B AA Spectrometer User’s Guide...

  • Page 16: Ultraviolet Radiation

    The beginning of the warning text is noted by a warning icon: WARNING A triangular symbol indicates a warning. The meanings of the symbols that may appear alongside warnings in the documentation or on the instrument itself are as follows: Agilent 55B AA Spectrometer User’s Guide...
  • Page 17 The following symbols appear on the instrument for your information. Mains power on Mains power off Fuse Single phase alternating current Agilent 55B AA Spectrometer User’s Guide...

  • Page 18: Ce Compliance

    Declaration of Conformity. The Declaration of Conformity is the legal declaration by Agilent that the product complies with the directives listed above, and shows the EN standards to which the product was tested to demonstrate compliance. Agilent 55B AA Spectrometer User’s Guide...

  • Page 19: Electromagnetic Compatibility

    Make sure that all peripheral devices are also certified. Make sure that appropriate cables are used to connect the device to peripheral equipment. Consult your equipment dealer, Agilent Technologies, or an experienced technician for assistance. Agilent 55B AA Spectrometer User’s Guide...

  • Page 20: Ices/Nmb-001

    When aspirating such solvents, always use a covered container and feed the capillary tubing through a 2 mm diameter hole in the cover. Always use the smallest volume of solvent consistent with your analytical requirements. Agilent 55B AA Spectrometer User’s Guide...
  • Page 21 Do not mix nitric or perchloric acid residues with organic solvent  residues. Keep the burner slot, spraychamber and liquid trap clean.  Always use the internal igniter to light the flame as its operation  indicates that all the safety interlocks are satisfied. Agilent 55B AA Spectrometer User’s Guide...

  • Page 22: Compressed Gases And Cylinders

    NEVER use any gas except acetylene as the fuel gas. Acetylene Unskilled, improper, or careless use of acetylene can create explosion hazards and fire hazards which can result in death, severe personal injury or burns. Agilent 55B AA Spectrometer User’s Guide...
  • Page 23 Use only acetylene that is packed in acetone with the Agilent 55B AA system. Some gas suppliers offer acetylene packed in material other than acetone. While these alternatives may overcome some of the...

  • Page 24: Nitrous Oxide

    Use only acetylene as the fuel gas. Use only air or nitrous oxide as oxidant. Never attempt to use oxygen or oxygen-enriched air, as this will cause a flashback. Agilent 55B AA Spectrometer User’s Guide...

  • Page 25: Nebulizer

    (e.g., a wire) to clean the capillary of a nebulizer while a flame is operating. ALWAYS extinguish the flame before removing the nebulizer from the nebulizer block. Regularly test all connections for leaks. Rectify all leaks before lighting the flame. Agilent 55B AA Spectrometer User’s Guide...

  • Page 26: Liquid Trap

    If you are not analyzing solutions of a toxic nature, leave the vapor outlet uncovered. Heat Hazards An open flame, burners and other hot surfaces can present heat hazards that can result in severe burns. Agilent 55B AA Spectrometer User’s Guide...

  • Page 27: Perchloric Acid

    Aspirate distilled water between samples. Minimize the  aspiration of air. Use separate spraychamber/liquid trap and drain assemblies for  perchloric acid analyses and organic solvent analyses to prevent perchloric acid from mixing with organic solvent residues. Agilent 55B AA Spectrometer User’s Guide...

  • Page 28: Flashbacks

    Agilent 55B AA Spectrometer User’s Guide...
  • Page 29 The end of the drain tube must not be allowed to drop below the level of the liquid in the vessel. (Conversely, the level of liquid must not be allowed to rise sufficiently to cover the end of the tube.) Agilent 55B AA Spectrometer User’s Guide...
  • Page 30 Failure to do this can result in unpredictable flashbacks. 10 Aspirating solutions (especially alkaline/ammoniacal ones) that contain high concentrations of Ag, Cu and Hg can lead to the formation of acetylides which can spontaneously decompose and cause a flashback. Agilent 55B AA Spectrometer User’s Guide...

  • Page 31: Introduction

    Specifications Environmental Specifications Gas Supplies The Agilent 55B AA (double beam) flame atomic absorption spectrometer combines minimal user setup and fast sample throughput with unparalleled ease of use. The instrument is controlled via a built-in keyboard and display, and can be upgraded by purchasing a PC and Agilent SpectrAA software (for more information, contact your local Agilent office).

  • Page 32: Site Preparation Requirements

    ‘Cookbook’ option). Bold text indicates the Keypad keys on your Agilent AA instrument (e.g., press the Read key). ALL CAPITALS indicates text you must type in from the keyboard (attached to an external PC). Agilent 55B AA Spectrometer User’s Guide...

  • Page 33: Specifications

    To maintain safety, only the UltrAA-lamp power supplies should be used at this connection. Front (lamp compartment) Deuterium lamp: Molex 3-way connection, behind lamp panel. WARNING Shock Hazard To maintain safety, only the deuterium lamp assembly should be used at this connection. Agilent 55B AA Spectrometer User’s Guide...

  • Page 34: Gas Supplies

    350 kPa (11 psi) (50 psi) (50 psi) Normal flow 0-10 13.5-20 11-16 rate (L/min) Adaptors are available Other gas connections Sample compartment: Push-on Air/N O connector for burner Push-on C connector for burner Agilent 55B AA Spectrometer User’s Guide...

  • Page 35: Installation

    Connect the components of the system to one another (see  ‘Connections’, Page 37) Connect the equipment to the power supply, and check the  setting of the two voltage taps (see ‘Power’, Page 38) Agilent 55B AA Spectrometer User’s Guide...

  • Page 36: Instrument Overview

    Figure 2. Front view of spectrometer 1. Chimney 2. Flame shield 3. Flame on/off buttons 4. Power on/off switch 5. Burner controls 6. Sample compartment front panel 7. LCD display 8. Keypad 9. Lamp compartment Agilent 55B AA Spectrometer User’s Guide...

  • Page 37: Connections

    RS-232 cable in the RS-232C 9-pin port at the rear of the instrument (upper left corner when viewed from the rear). If your printer is not a serial printer, you must use a serial to parallel converter. Agilent 55B AA Spectrometer User’s Guide...

  • Page 38: Power

    Guide. You should check the power requirements and read through the section ‘Electrical Power Supplies’ in the Site Preparation Guide before connecting the Agilent 55B AA system to the power supply. Consult the manuals supplied with your printer and PC (if required) for their power requirements.

  • Page 39: Moving Your Instrument

    The D lamp module is located within the lamp compartment, on the lower left hand side and is interlocked to prevent inadvertent exposure to hazardous UV radiation. Figure 3. Lamp compartment 1. D lamp compartment Agilent 55B AA Spectrometer User’s Guide...

  • Page 40: Hollow Cathode Lamps

    (see the following picture), and push the lamp into the socket, releasing the button as you push the lamp fully home. Hold the lamp by its base. Do not touch the quartz window at the end of the NOTE lamp. Agilent 55B AA Spectrometer User’s Guide...

  • Page 41: D 2 Lamp

    If you have this option, you will need to replace the D lamp approximately every 1000 hours of operation. For instructions on how to change a D lamp, refer to the Maintenance chapter. Agilent 55B AA Spectrometer User’s Guide...

  • Page 42: Sample Compartment

     spraychamber (see Page 45).  Figure 6. Nebulizer components (for products with serial numbers before 0110xxxx): 1. Nebulizer block 2. Nebulizer 3. Drain tube 4. Liquid trap 5. Float 6. Spraychamber Agilent 55B AA Spectrometer User’s Guide...
  • Page 43 The sensor is also designed to shut down the flame if the level falls below the required minimum during operation. Agilent 55B AA Spectrometer User’s Guide...
  • Page 44 (as described in ‘Reassembling the Nebulizer’, Page 103. Attach the spraychamber to the nebulizer block and install the complete assembly in the sample compartment (as described on Page 52. Agilent 55B AA Spectrometer User’s Guide...

  • Page 45: Spraychamber

    (sometimes referred to as the spraychamber  bung). Mixing Paddles The mixing paddles fit into the centre of the spraychamber. They remove the larger aerosol droplets which can cause photometric noise and burner blockage. Agilent 55B AA Spectrometer User’s Guide...
  • Page 46 Touching or otherwise contaminating any part of the mixing paddles will degrade NOTE the performance of the spraychamber. You must be careful to avoid contaminating the mixing paddles when handling them. For cleaning instructions, refer to the Maintenance chapter. Agilent 55B AA Spectrometer User’s Guide...
  • Page 47 To join the spraychamber and nebulizer block: Place the O-ring in the recess at the rear of the nebulizer block as shown in the following picture. Figure 9. O-ring in place in the nebulizer block Agilent 55B AA Spectrometer User’s Guide...
  • Page 48 NEVER attempt to light a flame with the drain tube missing. Refer to the following picture and insert the float (1) in the liquid trap. Figure 10. Top view of liquid trap showing correct placement of float Agilent 55B AA Spectrometer User’s Guide...
  • Page 49 Attach the liquid trap to the bottom of the nebulizer block by inserting the end of the plastic drain tube into the liquid trap and using a counter-clockwise twisting motion to engage the bayonet lock. Figure 11. Complete nebulizer/spraychamber assembly Agilent 55B AA Spectrometer User’s Guide...
  • Page 50 With the two vent nipples aligned with the nebulizer, lower the drain tube into the trap, ensuring that the float drops into the space between the two ribs that are opposite the two vent nipples. Refer to Figure 13. Agilent 55B AA Spectrometer User’s Guide...
  • Page 51 The explosion may be severe enough to cause death, personal injury or damage to the instrument or laboratory. NEVER attempt to light a flame unless the liquid trap is full. Agilent 55B AA Spectrometer User’s Guide...
  • Page 52 (the waste liquid must be allowed to drain freely into the waste vessel). The free end of the tubing must remain above the level of the liquid in the vessel. Agilent 55B AA Spectrometer User’s Guide...
  • Page 53 WARNING Fire and Explosion Hazard Failure to connect the vapor vent tubing correctly can cause a flashback or explosion. Ensure that the tubing is configured as described in the previous step. Agilent 55B AA Spectrometer User’s Guide...

  • Page 54: Burner

    Position the burner in the sample compartment, with the slot along the optical path and the plate with the warning towards the front of the instrument. Align the interlock key with the guide in the burner adjuster. Agilent 55B AA Spectrometer User’s Guide...

  • Page 55: Sample Compartment Front Panel

    Align the panel so that the two small holes fit over the two lugs on top of the burner adjuster, and lower the panel until it rests on the burner adjuster. Agilent 55B AA Spectrometer User’s Guide...

  • Page 56: Flame Shield

    To remove the flame shield, lift it up and unhook it from the front of the sample compartment. WARNING Hot Surface The chimney and flame shield may become very hot during operation and cause severe burns if touched. Always wear protective gloves when handling a hot chimney. Agilent 55B AA Spectrometer User’s Guide...

  • Page 57: Interface

    Navigating the Interface Changing Pages Selecting Menus Moving Between Fields This chapter provides an overview of the Agilent 55B AA user interface to help you become familiar with its various components. You should read through this chapter while exploring the interface. Introduction The Agilent 55B AA user interface consists of the following: Liquid Crystal Display—LCD...

  • Page 58: Display

    Interface Memory for storage of up to 30 customized methods.  Figure 15. Agilent 55B AA keypad and display area Display The display is divided into four areas: status area, signal bar, page area and message line, each of which is discussed below.
  • Page 59 It also informs you of the calibration status of the method. If the text “Cal” appears in the message line, the method has been calibrated. The text “Rslp” indicates the calibration has been resloped. No text (“ ”) indicates that the method has not been calibrated. Agilent 55B AA Spectrometer User’s Guide...
  • Page 60 Air-acetylene, no oxidant pressure Air only, oxidant pressure present Air only, no oxidant pressure Nitrous oxide-acetylene, oxidant pressure present Nitrous oxide-acetylene, no oxidant pressure Gas type icons are only displayed during times of other instrument activity. NOTE Agilent 55B AA Spectrometer User’s Guide...

  • Page 61: Keypad

    If the cursor is moved out of a field without Enter being pressed, the field’s NOTE contents returns to its previous value. Enter is also used on the Optimization page to perform a Rescale command (see Page 81). Agilent 55B AA Spectrometer User’s Guide...
  • Page 62 Calibration page ALT+Read Instrument zero Calibration page Reslope Perform reslope Calibration page ALT+Reslope Drop reslope standard Calibration page Read Take next reading Results page ALT+Read Instrument zero Results page Reslope Perform reslope Results page Agilent 55B AA Spectrometer User’s Guide...

  • Page 63: Agilent 55B Aa Pages

    The Instrument Parameters page is used to set the instrument parameters, and save and delete methods. The element can only be selected by loading an appropriate method (user or NOTE cookbook). This page includes the following instrument-specific fields: Agilent 55B AA Spectrometer User’s Guide...
  • Page 64 Defines the wavelength to be used for the current element (default is the first listed wavelength). The listed wavelengths are element and instrument-mode specific. NOTE Other λ Defines the wavelength to be used when ‘Other’ is selected in the Wavelength field. Range is 180.0–900.0. Agilent 55B AA Spectrometer User’s Guide...

  • Page 65: Measurement Parameters Page

    Identifies the next sample to be measured. This has no effect on the reading. Pre-read Delay Defines the time allowed for the sample to reach the light path and for the signal to stabilize. Read Time Defines the time for which the signal is measured. Agilent 55B AA Spectrometer User’s Guide...

  • Page 66: Options Page

    PROMT (PRecision Optimized Measurement Time) The signal is averaged until the desired precision (%RSD) is achieved or until the end of the ‘Read time’. When SIPS is being used set this value to 0.3%. NOTE Agilent 55B AA Spectrometer User’s Guide...
  • Page 67 Minimum Sample DF Defines the minimal sample dilution factor to be used. Primarily intended for where the majority of samples are suspected overrange. This will prevent unnecessary dilution factor changes, thus speeding up sample throughput. Agilent 55B AA Spectrometer User’s Guide...
  • Page 68 Defines the baud rate to be used for the serial port. Default is 9600. Lines Per Page Used when ‘Printer’ is selected as the text style (default is 66). Each page has a header. Form feeds are used to separate pages. Agilent 55B AA Spectrometer User’s Guide...

  • Page 69: Optimization Page

    0-3 decimal places. No two standards may have the same value, and they must be entered in increasing order. Entering a value of zero will delete the current and subsequent standards. Agilent 55B AA Spectrometer User’s Guide...

  • Page 70: Results Page

    The Precision column displays %RSD in Integration mode, %Pr in PROMT mode and remains blank in Integrate Repeat mode (with the heading %Pr). The Mean column always displays the mean reading for each solution. Agilent 55B AA Spectrometer User’s Guide...

  • Page 71: Navigating The Interface

    Up and Down keys to move from one item to the next, and, if necessary, press Enter to select the desired option. Figure 19. An example of a Command menu Agilent 55B AA Spectrometer User’s Guide...

  • Page 72: Moving Between Fields

    Moving Between Fields The cursor shows where the current focus is. When the cursor is on an entry field, the entire field is highlighted. To move between entry fields, use the Up/Down arrow keys. Agilent 55B AA Spectrometer User’s Guide...
  • Page 73 If Clr is pressed the entire field value is deleted. When Enter is pressed, the cursor moves to the next field (providing the value is valid). If the value entered is invalid, the cursor remains on the entry field and the value is not accepted. Agilent 55B AA Spectrometer User’s Guide...
  • Page 74 Interface This page is intentionally left blank. Agilent 55B AA Spectrometer User’s Guide...

  • Page 75: Operation

    Sample Measurement Results Shutting Down the System This chapter provides instructions for running your Agilent 55B AA instrument, including how to develop methods, optimize the system, perform measurements and print the results. This chapter assumes you have correctly installed the appropriate hardware as described in Chapter 3, and are familiar with the interface as described in Chapter 4.

  • Page 76: Starting The System

    When the initialization setup is complete the Load Method page is displayed. For instructions on how to start any accessories, refer to the manuals supplied with the accessories. Agilent 55B AA Spectrometer User’s Guide...

  • Page 77: Method Development

    ‘user’ method. To load a cookbook method: Press the Load Method button. Select the ‘Cookbook’ option. Select the appropriate element group. Select the required element from the list and press Enter. Agilent 55B AA Spectrometer User’s Guide...

  • Page 78: Setting The Instrument Parameters

    ‘Standby current’ for the standby lamp  whether ‘D correction’ is on or off  the ‘Gas type’  the ‘Wavelength’  the spectral bandwidth (the width of the ‘Slit’).  For more information, see Page 63. Agilent 55B AA Spectrometer User’s Guide...

  • Page 79: Setting The Measurement Parameters

    NOTE Parameters page is Conc5, which represents the concentration of the bulk standard. Conc1...4 are calculated from the bulk standard, and the Reslope standard is set at 3. For more information, see Page 90. Agilent 55B AA Spectrometer User’s Guide...

  • Page 80: Saving/Deleting Methods

    Move the highlight to the ‘Delete Method’ option and press Enter. Move the highlight to the method in the list you wish to delete and press Enter. The method will be deleted, leaving an empty slot in the list. Agilent 55B AA Spectrometer User’s Guide...

  • Page 81: Optimization

    Operation Optimization This section describes how to optimize the various components of the Agilent 55B AA system, including the lamp, burner and flame signal. Aligning Lamps Hollow Cathode Lamps If you are developing a new method, install the lamp and note the position, ensuring this position is setup in the method for that element.
  • Page 82 (refer to Page 109). If so, press Enter to Rescale. This will bring the signal back into range for display. You should also Rescale if the signal becomes too large. Repeat the previous step with the second D lamp adjustment knob. Agilent 55B AA Spectrometer User’s Guide...

  • Page 83: Aligning The Burner

    Prior to lighting the flame you must ensure that: the working area is completely clear of all hazardous materials  including corrosive liquids and flammable solvents the liquid trap is filled with an appropriate solvent  Agilent 55B AA Spectrometer User’s Guide...
  • Page 84 Check the gas regulator settings and readjust if necessary. When the flame has stabilized, adjust the flame conditions. Aspirate 50 mL of the appropriate solvent. When you are not aspirating a solution, you should be aspirating the appropriate solvent. Agilent 55B AA Spectrometer User’s Guide...

  • Page 85: Optimizing The Flame Signal

    You can find the optimum bead position for most applications by aspirating a 5 mg/L solution of copper. The system is now optimized. You can now take readings, measure your calibration standards, or perform a reslope as described in the following sections. Agilent 55B AA Spectrometer User’s Guide...

  • Page 86: Nebulizer Setup

    Loosen the locking ring and turn the ring and thimble fully clockwise. While nebulizing a suitable standard solution, observe the absorbance. Slowly and carefully turn the thimble counter- clockwise until the absorbance reaches a maximum. Agilent 55B AA Spectrometer User’s Guide...

  • Page 87: Low Vacuum Setting

    Fit the wide bore (0.64 mm ID) tubing to the capillary. Turn the locking ring clockwise until it is up against the nebulizer body. Turn the thimble clockwise as far as it will go. Agilent 55B AA Spectrometer User’s Guide...

  • Page 88: Setting The Uptake Rate For Organic Solvents

    Setting on Page 86, or if you are using organics, set the nebulizer to maximum uptake rate (thimble fully clockwise). Set the instrument up to measure the absorbance of copper in an air-acetylene flame. Agilent 55B AA Spectrometer User’s Guide...

  • Page 89: Calibrating The Method

    Define the standards to be used for the calibration as described on Page 79. Select the Cal Blank by moving the focus to the ‘Conc0’ field, then aspirate the blank and press the Read key. Agilent 55B AA Spectrometer User’s Guide...

  • Page 90: Measuring Standards Using Sips 10

    Parameters key in conjunction with the Alt key. The cross hairs on the graph can be moved using the arrow keys. The numbers displayed indicate the current signal and concentration of the location of the cross hairs. Agilent 55B AA Spectrometer User’s Guide...

  • Page 91: Resloping The Calibration

    On the Results page, press the Reslope key. The system will measure the reslope standard selected in the method and update the existing calibration. Cal Zero is not remeasured when a Reslope is performed. NOTE Agilent 55B AA Spectrometer User’s Guide...

  • Page 92: Sample Measurement

    Place the pump tubing in the appropriate sample and press the Read key. If the sample is overrange, SIPS automatically dilutes the sample online and measurement continues. The dilution factor used is given on the Results page and the final dilution-corrected concentration is reported. Agilent 55B AA Spectrometer User’s Guide...

  • Page 93: Results

    Each time the READ key is pressed data is output as follows: The layout is as follows: Calibration Standard ID, Concentration, Background Absorbance, Mean Absorbance, Replicates Absorbances. Batch Number, Sample Number, Concentration, Background Absorbance, Mean Absorbance, Replicates Absorbances. Agilent 55B AA Spectrometer User’s Guide...

  • Page 94: Shutting Down The System

    Turn off the instrument. Shut off all gas supplies at the regulators and gas cylinders. Empty the waste vessel. Turn off the exhaust fan. Remove and clean any hardware according to the instructions in the Maintenance Chapter. Agilent 55B AA Spectrometer User’s Guide...

  • Page 95: Maintenance

    Gas Supplies Lamp Fuses This chapter describes how to maintain your Agilent 55B AA system. You should keep a record in your Instrument Log Book of all maintenance carried out. Before you remove any hardware, you must shut down the instrument.

  • Page 96: Weekly

    If the windows are dirty, wipe them using an optical tissue held between plastic tweezers and dampened with a 50% ethanol/water solution. Agilent 55B AA Spectrometer User’s Guide...

  • Page 97: Filters

    To clean the burner: Remove the chimney, flame shield and sample compartment front panel from the instrument. Remove the burner from the spraychamber by lifting the burner assembly upwards. This may require a slight twisting motion. Agilent 55B AA Spectrometer User’s Guide...
  • Page 98 Rinse the burner thoroughly, preferably in the ultrasonic bath again, to remove all traces of the polish. 10 Dry the burner and inspect it under the microscope. Agilent 55B AA Spectrometer User’s Guide...

  • Page 99: Nebulizer

    Regularly (monthly) remove and check the nebulizer as described  below, then re-install the nebulizer (as described in Chapter 3) and measure the uptake rate (as described in Chapter 5). Agilent 55B AA Spectrometer User’s Guide...

  • Page 100: Removing The Nebulizer Block

    Remove the liquid trap by holding the nebulizer/spraychamber assembly firmly in one hand, and twisting the liquid trap in a counter-clockwise direction to unlock the bayonet mount. Unscrew the plastic drain tube from the bottom of the nebulizer block. Agilent 55B AA Spectrometer User’s Guide...

  • Page 101: Disassembling The Nebulizer

    To do this, slacken the clamping screw that secures the impact bead in the adjuster block, and move the impact bead to the side (see Page 104 if necessary). Agilent 55B AA Spectrometer User’s Guide...

  • Page 102: Cleaning A Blocked Nebulizer

    After cutting off the clogged section, it may be necessary to ‘flare’ the end of the capillary before it can be fitted to the nebulizer. You may do this with a heated needle. Agilent 55B AA Spectrometer User’s Guide...

  • Page 103: Reassembling The Nebulizer

    Do not over-tighten. Carefully guide the locking thimble and ring over the capillary and screw it onto the nebulizer body. You may need to push it in slightly before the threads will catch. Agilent 55B AA Spectrometer User’s Guide...

  • Page 104: Impact Bead

    (approximately two turns), as shown in the following picture. Figure 24. Nebulizer block 1. Flat-blade screw driver 2. Clamping screw 3. Impact bead adjuster block Remove the impact bead from the nebulizer block, using a twisting motion if necessary. Agilent 55B AA Spectrometer User’s Guide...
  • Page 105 If the adjuster block is difficult to remove due to broken glass trapped in the bead, use a piece of wire or similar to pry the broken glass out from the cavity in the nebulizer block. Agilent 55B AA Spectrometer User’s Guide...
  • Page 106 The impact bead adjuster block must be positioned as close as possible to the NOTE front of the nebulizer block, as shown above. This will avoid breaking the impact bead when a new one is installed. Agilent 55B AA Spectrometer User’s Guide...

  • Page 107: Installing And Adjusting The Impact Bead

    Gradually turn the impact bead adjuster first clockwise, then anticlockwise until the signal is at a maximum. The reduced sensitivity setting is obtained by turning the impact bead adjuster clockwise until the signal is about 40% of the maximum signal. Agilent 55B AA Spectrometer User’s Guide...

  • Page 108: Spraychamber

    Rinse all parts thoroughly with distilled water and dry thoroughly. Inspect all O-rings and replace any that are cracked or deformed. Replacement is easier if the O-rings are wetted with distilled water. Reassemble the spraychamber according to the instructions in Chapter 3. Agilent 55B AA Spectrometer User’s Guide...

  • Page 109: Gas Supplies

    Agilent field service engineer for advice. WARNING Hot Surface The D lamp and its cover become very hot during operation. To prevent skin burns, allow the assembly to cool down before removing it. Agilent 55B AA Spectrometer User’s Guide...
  • Page 110 (3) as in Figure 27. Figure 27. D lamp alignment (top view) Refer to Figure 28 and rotate the lamp so that the face with the aperture (1) is parallel with the top edge of the bracket (2). Agilent 55B AA Spectrometer User’s Guide...

  • Page 111: Fuses

    (‘T’= time lag, ‘F’= fast acting), the current rating (in amperes), the breaking capacity (‘H’= heavy, ‘L’= low) and the voltage rating (in volts). This code must correspond to the code appearing next to the fuseholders. Agilent 55B AA Spectrometer User’s Guide...
  • Page 112 (1) to lever the fuse holder (2) from the instrument. Check that the fuses are the correct type and are not damaged. If necessary, replace the fuses. Agilent 55B AA Spectrometer User’s Guide...
  • Page 113 If a fuse blows repeatedly, it may indicate other problems with the Agilent 55B NOTE AA instrument. You should contact your local Agilent sales office and arrange a service call. Agilent 55B AA Spectrometer User’s Guide...
  • Page 114 Maintenance This page is intentionally left blank. Agilent 55B AA Spectrometer User’s Guide...

  • Page 115: Spare Parts

    Sample Introduction Other Covers/Doors Fuses Miscellaneous This chapter contains information for your Agilent 55B AA spare parts. Unless otherwise specified, only Agilent supplied parts should be used. See the Agilent website for part number and ordering information at www.agilent.com Sample Introduction Figure 29.
  • Page 116 14 O-ring, nitrile O-ring, organics 15 Spraychamber, molding fluorinated 16 Mixing paddles 17 Pressure relief bung 18 O-ring, pressure relief bung, nitrile O-ring, pressure relief bung, organics 19 Air/acetylene burner, Mark 7 0/acetylene burner, Mark 7 Agilent 55B AA Spectrometer User’s Guide...
  • Page 117 Figure 32. Various components from the nebulizer block 20 Glass impact bead (packet of 5) 21 Clamp bead adjuster 22 Impact bead locking screw (PEEK) 23 Trapping screw (stainless steel) 24 Plug grey PEEK 25 O-ring 3/16 in. ID Agilent 55B AA Spectrometer User’s Guide...

  • Page 118: Other

    Miscellaneous Drip tray Chimney Serial to parallel converter 240 V 110 V SpectrAA mouse mat Kit Agilent AA keyboard overlays Includes overlays in French, German, Italian and Spanish Kit spraychamber stand Remote read footswitch Agilent 55B AA Spectrometer User’s Guide...

  • Page 119: Troubleshooting/Errors

    Check nebulizer is correctly assembled and adjusted. c) Check for leaks. Flame sensed with no flame a) Too much light in the sample compartment. Ensure chimney and flame shields are fitted. Turn off nearby lights. b) Flame sensor faulty. Agilent 55B AA Spectrometer User’s Guide...
  • Page 120 Check for chemical interference. e) Check fuel to oxidant ratio is correct. f) Check burner is clean and clear of deposits. g) Check solutions have not expired. h) Check wavelength selection and calibration. Agilent 55B AA Spectrometer User’s Guide...
  • Page 121 19 Signal not increasing and a) Check standard solutions (particularly high standard). excessive curvature b) Select a different wavelength. c) Reduce lamp current. d) Reduce slit width. e) Operate within the working range (0.1 to 0.8 Abs). Agilent 55B AA Spectrometer User’s Guide...

  • Page 122: Error Messages

    (Laboratory Information Management System) via the serial RS-232C port. 2851 SIPS comms error There has been a communication problem with the SIPS sample introduction pump unit. Check all cables to this unit are connected securely. Agilent 55B AA Spectrometer User’s Guide...

  • Page 123: 3800 Eeprom Storage Error

    5008 Reslope signal out of range Reslope calibration has failed. The reslope standard signal reading was too far out to be used. (The Reslope signal value cannot differ from the original value by more than 25%.) Agilent 55B AA Spectrometer User’s Guide...

  • Page 124: 6000 Check Hc Lamp Selection

     If the error persists, a service call may be required. 9308 RBC/Mains frequency The instrument detected a power mains supply fault: Mains frequency out of range. Possible causes include: Power supply failure  Agilent 55B AA Spectrometer User’s Guide...

  • Page 125: 9309 Rbc/Mains Frequency Above 62Hz

    Instrument Fault. The instrument detected a problem with the -12 volt supply. A service call may be required. 9313 Instrument Fault 5V PSU Instrument Fault. The instrument detected a problem with the 5 volt supply. A service call may be required. Agilent 55B AA Spectrometer User’s Guide...

  • Page 126: 9316 Wavelength Out Of Range

    The instrument Gain had been set to its lowest value but the hollow cathode lamp signal was too high. Possible causes include: Hollow cathode lamp misaligned  Faulty hollow cathode lamp  Faulty PMT or related circuits.  Agilent 55B AA Spectrometer User’s Guide...

  • Page 127: 9319 No Peak: Low Bc Lamp Energy

    Faulty hollow cathode lamp.  Suggested action: Check that the optical light path is not obstructed in the sample compartment. Exit then re-enter the Optimize page/window. This will cause the instrument to retry the peaking. Agilent 55B AA Spectrometer User’s Guide...

  • Page 128: 9322 No Peak: High Hc Lamp Energy

    The instrument Gain had been set to its lowest value but the signal was too high. Possible causes include: Emission Setup has not been performed  Wrong wavelength selected  Faulty PMT or related circuit  Agilent 55B AA Spectrometer User’s Guide...

  • Page 129: 9329 No Peak Detected

    Wrong wavelength or method selected  Slit width (SBW) selection incorrect  The lamp position in the method is incorrect.  A wavelength correction fault. The error 9621 Instrument Fault: Wl correction occurred prior to this error. Agilent 55B AA Spectrometer User’s Guide...

  • Page 130: 9337 Instrument Fault 310V Psu

    The instrument could not detect any lamp current for the selected hollow cathode lamp. Possible causes include: No hollow cathode lamp is installed in the selected lamp position  Faulty hollow cathode lamp  Faulty lamp supply circuits.  Agilent 55B AA Spectrometer User’s Guide...

  • Page 131: 9514 Instrument Signal Saturation

    Possible causes include: Hollow cathode lamp misaligned  Faulty hollow cathode lamp  Faulty PMT or circuits  The lamp was in the wrong position when the instrument was  optimized. Agilent 55B AA Spectrometer User’s Guide...

  • Page 132: 9524 Low Bc Lamp Energy

    ) lamp. No lamp current has been detected and the D lamp has been presumed faulty. Change the D lamp as described in Chapter 6. If the problem persists a service call may be required. Agilent 55B AA Spectrometer User’s Guide...

  • Page 133: 9529 Background Lamp Interlock

    Restart the instrument. If the problem persists a service call will be required. 9911 No Burner Fitted An attempt was made to ignite the flame without any burner installed in the sample compartment. Agilent 55B AA Spectrometer User’s Guide...

  • Page 134: 9912 N O Burner Not Fitted

    This error may also be returned while running in Air Only mode. Possible causes include: Air or N O gas cylinders empty or turned off  Faulty pressure sensor  Faulty gas supply regulation.  Agilent 55B AA Spectrometer User’s Guide...

  • Page 135: 9920 Fault: Flame Detected

    Wait at least 4 seconds for the gases to disperse, then try again. Possible causes include: The acetylene gas cylinder is empty or turned off  The fuel flow is too low (only on the MANUAL gas box)  The igniter failed.  Agilent 55B AA Spectrometer User’s Guide...

  • Page 136: 9934 Flame Shutdown: Host Offline

    Agilent field service engineer. 9xxx SpectrAA Error This is an internal instrument error and should not occur. Record the actual error number (e.g. 9903). Restart the instrument. If the error persists contact your Agilent field service engineer. Agilent 55B AA Spectrometer User’s Guide...
  • Page 138 The guide describes the following: Safety Practices and Hazards  Introduction  Installation  Interface  Operation  Maintenance  Spare Parts  Troubleshooting and Errors  © Agilent Technologies 1997, 2000, 2002, 2009-2010, 2012-2013, 2016- 2017 12/17 *8510154100* *8510154100* 8510154100 Issue 12...

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