GBC SavantAA No Flame Operation Manual

GBC SavantAA No Flame Operation Manual

Atomic absorption spectrometer
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AAS
AAS
SAVANTAA
OPERATION MANUAL
Part No. 01-0996-01

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Summary of Contents for GBC SavantAA No Flame

  • Page 1 SAVANTAA OPERATION MANUAL Part No. 01-0996-01...
  • Page 2 GBC Scientific Equipment Pty Ltd. GBC Scientific Equipment Pty Ltd assumes no responsibility for any errors that may appear in this document or any damages arising out of the use or inability of this document.
  • Page 3: Table Of Contents

    Table of Contents GBC SavantAA Operation Manual...
  • Page 4: Table Of Contents

    Intended use of the instrument ....................16 Instrument positioning ......................16 Safety signs ..........................16 Warning ..........................16 Electrical hazard ........................16 Electrical hazards........................16 Fuse replacement ........................ 16 High voltages ........................16 Earthing requirement ......................17 GBC SavantAA Operation Manual...
  • Page 5 The software modules ....................... 34 File saving ........................... 34 Method ..........................34 Samples ..........................34 Analysis ..........................35 Results ..........................36 Report ..........................37 Instrument ........................... 38 On-line help system ........................38 On-line help conventions...................... 39 GBC SavantAA Operation Manual...
  • Page 6 Extinguishing the flame ......................64 Gas flow optimisation for programmable flame control ............64 Optimising gas flow rates...................... 64 Nebuliser optimisation......................65 Impact bead ........................65 Optimising the burner angle ....................66 Automatic burner rotation (ABR) – optional ................66 GBC SavantAA Operation Manual...
  • Page 7 PAL furnace auto sampler ......................85 Unpacking ........................... 85 Connections......................... 85 GF5000 power up ........................ 86 Setting the probe tip position ....................86 FURNACE ANALYSIS TUTORIAL..................89 Instrument configuration ......................90 Lamp installation ........................91 Installing other lamps ......................91 GBC SavantAA Operation Manual...
  • Page 8 Bleeding gas lines ........................ 98 Nebuliser removal/replacement .................... 98 Impact bead adjustment ...................... 99 Nitrous oxide-acetylene burner cleaning ................100 Graphite furnace........................100 Furnace tube removal/replacement ..................100 PAL auto sampler........................101 Syringe removal/replacement ..................... 101 Syringe trouble-shooting..................... 102 GBC SavantAA Operation Manual...
  • Page 9: About This Manual

    About this manual About this manual This manual provides installation and operating instructions for the GBC SavantAA Atomic Absorption Spectrometer and accessories, including auto samplers and furnace system. The manual also contains two tutorials, which are of particular benefit to all users, regardless of their level of experience.
  • Page 10: Graphite Furnace (System 5000) And Furnace Analysis Tutorial

    This chapter outlines the routine maintenance requirements necessary for the instrument to remain in optimum condition. Using this manual When using this manual, GBC recommends the following: If you are a first time AA user: Ensure that you familiarise yourself with the basic operating procedures of the instrument, such as installing and optimising the lamps and igniting the burner (outlined in the chapters on pages 43 and 51).
  • Page 11: Introduction

    Introduction GBC SavantAA Operation Manual...
  • Page 12: Equipment Overview

    Beam Automatic NOTE: Model SavantAA No Flame and SavantAA Z enduro are configured for operation with a graphite furnace and are not capable of flame operation. SavantAA accessories The SavantAA spectrophotometers are compatible with a full range of accessories, including graphite furnaces, auto samplers and hydride/vapour generation systems.
  • Page 13: System 5000 Graphite Furnace

    A longer collection time translates to a higher measured signal. This accessory is ideal where pre-concentration of mercury is required for samples with very low mercury concentrations. GBC SavantAA Operation Manual...
  • Page 14: Other Accessories

    • Printers (which connect to the computer). • Hollow Cathode Lamps for 69 elements. • Super Lamps, which utilise the built-in power supply. • Installation accessories such as compressors, fume extraction systems and gas regulators. GBC SavantAA Operation Manual...
  • Page 15: For Your Safety

    For your safety GBC SavantAA Operation Manual...
  • Page 16: Intended Use Of The Instrument

    High voltages The SavantAA electronics uses dangerous voltages. The instrument should be serviced only by service personnel trained by GBC staff and holding a GBC Service Training certificate. GBC SavantAA Operation Manual...
  • Page 17: Earthing Requirement

    The GBC representative is responsible to ensure that the connectors and line types used conform to the national requirements. The GBC representative is responsible to carry out leak tests of the gas hoses connected to the equipment on installation and during yearly maintenance operations.
  • Page 18: Acetylene

    Never pipe acetylene in copper pipes, instead use stainless steel. Brass fittings should have less than 65% copper content. Fittings supplied by GBC are safe. If you have any doubts about other fittings consult your gas supplier.
  • Page 19: Flammable Samples

    The liquid trap should be filled with the liquid used for standards and samples preparation. The liquid trap should drain into an open plastic container. Never use a glass bottle. Further liquid trap set-up details are given on page 53. GBC SavantAA Operation Manual...
  • Page 20 For your safety This page is left blank intentionally GBC SavantAA Operation Manual...
  • Page 21: Instrument Installation

    Instrument installation GBC SavantAA Operation Manual...
  • Page 22: Introduction

    This entails ensuring the instrument is in a suitably ventilated or air- conditioned room, as well as following good laboratory practice in the handling and storage of chemicals. GBC accepts no responsibility for damage or lack of performance due to poor operating conditions.
  • Page 23: Location

    The overall dimensions of each SavantAA instrument are: Width: 950 mm Depth: 600 mm Height: 500 mm Computer SavantAA GF5000 Printer monitor (optional) Keyboard Auto Sampler Figure 1: Recommended bench for a full SavantAA AAS system GBC SavantAA Operation Manual...
  • Page 24: Exhaust Requirements

    A fume extraction accessory (including a damper control) is available from GBC (Part No. 99-0012-00 (220/240 V, 50 Hz), 99-0012-01 (110 V, 60 Hz), or 99-0400-00 (220 V, 60 Hz)). Please direct any enquiries to your dealer.
  • Page 25: Acceptable Instrument Inlet Pressure Ranges

    The instrument you have just unpacked may have been transported an extremely long distance. You should check for any damage that may have occurred during transit. Notify your dealer immediately if there are any problems. GBC SavantAA Operation Manual...
  • Page 26: Connections

    Set up your computer, monitor, keyboard, printer and mouse according to the instructions supplied with this equipment. Then make the following connections: Gas supply lines for air, nitrous oxide (if used), and acetylene (refer to the diagram below). Figure 3: Gas connections to the SavantAA GBC SavantAA Operation Manual...
  • Page 27: Installing Specific Components

    The Graphite Furnace (System 5000) chapter on page 81 outlines instructions for the installation of the components of the System 5000 graphite furnace, including the GF5000 power supply and furnace workhead, and the PAL furnace auto sampler. GBC SavantAA Operation Manual...
  • Page 28 Instrument installation This page is left blank intentionally GBC SavantAA Operation Manual...
  • Page 29: Savantaa Software

    SavantAA software GBC SavantAA Operation Manual...
  • Page 30: Introduction

    Enter to accept the highlighted option. Selecting items via the mouse Selecting items using the mouse can be achieved by placing the mouse pointer over the appropriate button or area and pressing the left mouse GBC SavantAA Operation Manual...
  • Page 31: Installing The Software

    Connect the USB cable provided between the computer and the SavantAA. Each end of the cable is different to the other. Insert the GBC SavantAA AAS software CD into the CD drive. The computer operating system must be Windows ®...
  • Page 32: Selecting The Hardware Setup

    Click NEXT. • Ready to Install. Click NEXT. • Completing the GBC SavantAA Setup Wizard. If you have chosen Launch the software opens when you click Finish. o Click FINISH. Open the Software or if you have chosen “Launch” after software installation, it automatically opens when the software installation is finished.
  • Page 33 Figure 6: An instrument screen showing the base model SavantAA system Figure 7: An instrument screen showing a SavantAA system with a HG3000 and SDS720 installed GBC SavantAA Operation Manual...
  • Page 34: The Software Modules

    The list of options for measurement type include Calibration, Rescale, Check Sample, Sample and Spike and Sample Blank. These options can be accessed by double clicking on a cell within the Measurement Type column. GBC SavantAA Operation Manual...
  • Page 35: Analysis

    (accessed from the pop-up menu displayed when you click on the right mouse button). If you choose the multiple analysis option, a table is displayed where the method, sample and results files for each analysis can be entered. Figure 10: Analysis module screen GBC SavantAA Operation Manual...
  • Page 36: Results

    Also displayed on the screen is a Status Panel: Status panel Displays the running absorbance and concentration. The data for each measurement is appended to the list shown in the List Window as it is GBC SavantAA Operation Manual...
  • Page 37: Report

    Analysis data to be included in the report is selected from the Results mode. Figure 12: Report module screen GBC SavantAA Operation Manual...
  • Page 38: Instrument

    The additional convenience of using the F1 key is that it is context- sensitive to the six modules and to the property sheets within the six modules. For example, if you are in the Description Property sheet within GBC SavantAA Operation Manual...
  • Page 39: On-Line Help Conventions

    Once you are in the On-line Help system, you can search for a topic of interest in a number ways. Topics Choosing the Topics option from the Help menu displays a screen containing two ways to search for help—Contents or Index. GBC SavantAA Operation Manual...
  • Page 40 Enter. A Help topic is indicated by an icon showing a page. To display the Help topic, click on the icon or highlight the topic and press Enter. Figure 14: Help contents page GBC SavantAA Operation Manual...
  • Page 41 You can scroll through these topics to find the area of interest using the arrow buttons at the top of the screen. GBC SavantAA Operation Manual...
  • Page 42 SavantAA software This page is left blank intentionally GBC SavantAA Operation Manual...
  • Page 43: Installing And Optimising Lamps

    Installing and optimising lamps GBC SavantAA Operation Manual...
  • Page 44: Installing Lamps

    Installing and optimising lamps The GBC SavantAA range all come standard with an automatically aligning and peaking eight-lamp turret. Installing lamps The SavantAA has an eight-lamp turret which is completely controlled by the computer. Lamp selection, optimisation (peaking) and warm-up (during multi-element operation) are all automated, ensuring optimal lamp operating conditions for the analysis.
  • Page 45 Figure 19: Open the retaining clip to Figure 20: Engage the key, then slide the admit the lamp, then fully release it gently lamp sideways to engage it in the socket Figure 21: The fully installed lamp GBC SavantAA Operation Manual...
  • Page 46: Additional Lamps

    If the SavantAA is fitted with a built-in Super Lamp power supply it will be in position 1 for a single Super Lamp power supply. Turret positions 3, 5 and 7 can also be configured for accepting Super Lamps. This is achieved using a four-lamp Super Lamp power supply. GBC SavantAA Operation Manual...
  • Page 47: Optimising Lamps

    60–300 seconds (1–5 minutes). These are manually entered. Open the Element Lamp Table. In the Stabilisation Delay window type the desired time interval in seconds and press Enter or click OK. The valid range is 0–9999 minutes. GBC SavantAA Operation Manual...
  • Page 48: Deuterium Lamps

    Install at least one hollow cathode lamp, update the Element Lamp Table, and ensure that the element is entered in the Description page of the Method module. Power up the instrument. If necessary, lower the burner so that it is below the light path. GBC SavantAA Operation Manual...
  • Page 49 HC lamp will cause the HC lamp meter to drop to zero. Click the button in the top right corner of the HC + D Alignment window to return to the Instrument screen. GBC SavantAA Operation Manual...
  • Page 50 Installing and optimising lamps This page is left blank intentionally GBC SavantAA Operation Manual...
  • Page 51: Flame Atomisation System

    Flame atomisation system GBC SavantAA Operation Manual...
  • Page 52: Savantaa Flame Atomisation System With Automatic Burner Rotation

    If the instrument is a SavantAA Σ or has the optional automatic workhead adjuster for other SavantAA models then it will not have the vertical and horizontal burner adjuster knobs, but everything else will be the same as the picture below. GBC SavantAA Operation Manual...
  • Page 53: Liquid Trap/Spray Chamber

    Figure 24 (or Figure 25 if ABR is fitted), complete with interlock connectors inserted. However, before the system can be used, the integral liquid trap must be readied for operation as detailed below: GBC SavantAA Operation Manual...
  • Page 54: Filling The Liquid Trap

    SavantAA. Spray chamber/liquid trap removal/replacement This section describes how to remove (and replace) the complete burner/spray chamber/nebuliser/liquid trap assembly from the sample compartment. This is required before setting up the instrument for graphite furnace analysis. GBC SavantAA Operation Manual...
  • Page 55 Firmly push the unit until the back of the spray chamber is flush against the mounting plate, and then tighten the two Allen screws with the supplied hex ball driver. Reconnect the liquid trap drain hose. Reconnect the spray chamber/liquid trap and burner interlock connectors. GBC SavantAA Operation Manual...
  • Page 56: Burners

    Each burner has a three-lug bayonet fitting which allows rapid burner removal and replacement. Burner rotation is an integral feature of GBC burners, offering maximum sensitivity reduction. The top part of the burners used in all instruments is exactly the same. The base of the burner differs between the standard flame systems and the ABR systems.
  • Page 57: Burner Cleaning

    The required wavelength and slit width for the current application will first be set. The turret will automatically move the required lamp into position and set the lamp current, lamp vertical and horizontal position and EHT. GBC SavantAA Operation Manual...
  • Page 58: Optimising The Burner Position

    Standard solution. In this case, optimisation of the vertical control will be less critical than the horizontal and rotational controls, since these two affect the path length of the absorbing sample. This process is described on pages 64–65. GBC SavantAA Operation Manual...
  • Page 59: Motorised Vertical Only Movement Burner (Mvom) Option

    Once an optimum absorbance is obtained these parameters can be saved in the method so that each time the method is used the optimal parameters will be used. GBC SavantAA Operation Manual...
  • Page 60: Programmable Flame Control

    The flame cannot be ignited if the nebuliser or pressure relief bungs are not installed or are not gas-tight. • If the mains power should fail, an auxiliary power supply allows the system to follow the normal flame shutdown sequence. GBC SavantAA Operation Manual...
  • Page 61: Gasbox Status

    Not Ready Flame cannot be ignited due to the condition of at least one interlock. See the list below. Waiting on Instrument Instrument busy or not communicating. Gasbox not responding Gasbox not communicating. GBC SavantAA Operation Manual...
  • Page 62: Interlock Status

    The spray chamber was not gas-tight. Integrity Check for the presence of burner, nebuliser and pressure relief bung, and if the interlock plug is inserted. If all are installed, check the o-rings and the seating of bungs. GBC SavantAA Operation Manual...
  • Page 63: Last Shutdown

    Ensure there are no flammable liquids in the vicinity of the burner compartment of the instrument. Make sure the pressure relief bung is in place. Ensure that Flame is selected as the System Type (Instrument Properties). GBC SavantAA Operation Manual...
  • Page 64: Igniting The Burner Flame

    Select and activate the Gas Flows Optimisation status panel by double clicking on the flame in the Instrument module, or press the Optimise button on the flame page of the method. This displays a meter calibrated to read absorbance (or emission), and six bar meters (for GBC SavantAA Operation Manual...
  • Page 65: Nebuliser Optimisation

    Unscrew the grub screw on the front face of the nebuliser bung a few turns using the 1.5 mm hex key supplied. Gently push the glass impact bead fully in until it just touches the end of the nebuliser. GBC SavantAA Operation Manual...
  • Page 66: Optimising The Burner Angle

    Optimising the zero position for normal samples The burner should first be aligned along the light path for applications requiring a maximum path length flame (nominal 0.0° angle). The optimum angle may not necessarily be 0.0°. GBC SavantAA Operation Manual...
  • Page 67: Optimising The Burner Angle For Over-Range Samples

    Typically the highest concentration standard from the first angle will be the lowest concentration standard for the second angle etc. Ensure that a calibration is run at the selected angle before measuring samples (either before or during the run). GBC SavantAA Operation Manual...
  • Page 68 Flame atomisation system This page is left blank intentionally GBC SavantAA Operation Manual...
  • Page 69: Sds720 Auto Sampler

    SDS720 auto sampler GBC SavantAA Operation Manual...
  • Page 70: Description

    Measure and terminate the sample tubing between the probe and the nebuliser. If necessary, adjust the height of the sampler probe to ensure adequate clearance above the test tube as per instructions in the manual. GBC SavantAA Operation Manual...
  • Page 71: Aspiration Tube

    Always aspirate distilled water after use to ensure that the aspiration tube and spray chamber are clean. • Always clean up spills as soon as they occur to prevent possible damage to the carousel cover. • Never retard the movement of the probe arm. GBC SavantAA Operation Manual...
  • Page 72 SDS720 auto sampler This page is left blank intentionally GBC SavantAA Operation Manual...
  • Page 73: Flame Analysis Tutorial

    Flame analysis tutorial GBC SavantAA Operation Manual...
  • Page 74: Lamp Selection

    This analysis will be performed in manual mode without an auto sampler. Therefore ensure that the radio button for No Sampler is selected in the Accessories section found on the same page. Refer to Figure 30 on page 75. GBC SavantAA Operation Manual...
  • Page 75 Return to the Instrument module, then right click and select Properties. Select the Element Lamp Table tab. Cu appears in the Element Lamp Table in the position corresponding to the number where it has been installed. GBC SavantAA Operation Manual...
  • Page 76: Method Development

    Element field or by clicking on the arrow next to the Element field and selecting the element from the periodic table. When the element is selected the turret will automatically rotate to the correct position. GBC SavantAA Operation Manual...
  • Page 77 The gas flow rates and the burner angle and height are controlled from the Flame Control page. Numerical values can be entered but it is better if the system is optimised for the particular element to be analysed. To do this, click on the Optimise button. GBC SavantAA Operation Manual...
  • Page 78 Click on the Samples button. Double click on the first row under the measurement column and select Calibration. Press the tick button . A calibration will now be displayed as the first measurement then insert three samples using the Add Row icon on the bottom toolbar. GBC SavantAA Operation Manual...
  • Page 79: Performing An Analysis

    Print icon. If you want to print just the results from one analysis then right click anywhere in that analysis and select Print Analysis. GBC SavantAA Operation Manual...
  • Page 80 Flame analysis tutorial This page is left blank intentionally GBC SavantAA Operation Manual...
  • Page 81: Graphite Furnace (System 5000) Installation

    Graphite furnace (System 5000) installation GBC SavantAA Operation Manual...
  • Page 82: Gf5000 Controls

    The auxiliary gas can be then set for the required low flow and selected during the atomisation. The auxiliary option can be used to supply clean compressed air during the ash stage. GBC SavantAA Operation Manual...
  • Page 83: Water Requirements

    Connect the in-built mains power cable to the power outlet. Optimisation of light paths If you have not already done so, follow the procedures for optimising the deuterium lamp given in the Installing and Optimising Lamps chapter on page 48. GBC SavantAA Operation Manual...
  • Page 84: Workhead Installation

    Properties, and then select the Configuration tab. The following screen is displayed. Figure 33: Instrument properties configuration showing furnace selections Select Furnace and then click on OK. Double click on the furnace workhead. The following status panel is displayed: GBC SavantAA Operation Manual...
  • Page 85: Pal Furnace Auto Sampler

    Connect the in-built communications cable to the connector at the rear of the GF5000. Connect the drain tube to the drain connector on the PAL base. Connect the thinner tube from the rinse bottle to the inlet on the sampler. GBC SavantAA Operation Manual...
  • Page 86: Gf5000 Power Up

    PAL Probe Tip Setup status panel will be displayed. The PAL will perform a simulated injection, with the sampler arm stopping at its currently programmed (default) injection position. Figure 35: PAL probe tip setup status panel GBC SavantAA Operation Manual...
  • Page 87 Use the ESV camera or supplied mirror to check the insertion depth. Any blocking of the light path by the capillary will be indicated by a corresponding increase in absorbance on the meter. Close the status panel. This returns the sampler arm to the Flush position. GBC SavantAA Operation Manual...
  • Page 88 Graphite furnace (System 5000) installation This page is left blank intentionally GBC SavantAA Operation Manual...
  • Page 89: Furnace Analysis Tutorial

    Furnace analysis tutorial GBC SavantAA Operation Manual...
  • Page 90: Instrument Configuration

    Accessories field found on the same page is checked by clicking on it. • Click on the OK button. Only the SavantAA with a System 5000 and PAL auto sampler should be displayed on the screen. Figure 36: Instrument properties configuration page showing correct selections GBC SavantAA Operation Manual...
  • Page 91: Lamp Installation

    The above is for illustrative purposes only. The actual position where the Pb lamp is entered will depend on the position at which it was installed. Similarly for the Stabilisation Delay times enter 0.00. • When finished click on the OK button to return to the Instrument module. GBC SavantAA Operation Manual...
  • Page 92: Deuterium Lamp Alignment

    Type any text for the Conc Units such as ppb or μg/L. Enter 2 in the Decimal places field to enable the results to be reported to two decimal places. Select Stop for the Cal. Failure Action field. GBC SavantAA Operation Manual...
  • Page 93 Indicates the read step. There is only one read step per furnace program. A graph: Indicates that the signal graphics to be shown for this step. The user can select the steps (none to all) where signal graphics are to be displayed. GBC SavantAA Operation Manual...
  • Page 94 Sample Preparation select Autocalc. Click OK. Go to the Sample Prep page to setup the PAL auto sampler parameters. On the Volume tab enter the following values: Enter 10 for the Sample Volume (μL) Enter 0 for the Modifier Volume (μL) GBC SavantAA Operation Manual...
  • Page 95: Performing An Analysis

    Return to the Results module. If you wish to print the results from all of the analyses contained in this results file then click on the Print icon. If you want to print just the results from one analysis then right click anywhere in that analysis and select Print Analysis. GBC SavantAA Operation Manual...
  • Page 96 Furnace analysis tutorial This page is left blank intentionally GBC SavantAA Operation Manual...
  • Page 97: Maintenance

    Maintenance GBC SavantAA Operation Manual...
  • Page 98: Optics

    Maintenance Maintenance procedures should only be attempted by suitably experienced personnel. The following procedures may be undertaken by experienced operators. If in doubt, call your GBC Service Representative. Optics Deuterium lamp removal/replacement To remove the deuterium (D ) lamp: Open the lamp compartment door.
  • Page 99: Impact Bead Adjustment

    Replace the grub screw in the threaded hole on the front face of the nebuliser bung. Stop as soon as you feel it touch the end of the impact bead. Place silicon sealant over the end of the bead-setting threaded hole to make it gas-tight. GBC SavantAA Operation Manual...
  • Page 100: Nitrous Oxide-Acetylene Burner Cleaning

    (containing distilled water). Any particles lodged in the slot can be removed with a cardboard card such as the GBC Burner Cleaning Card (Part No. 04-0032-00, pack of 20) or a business card. (Do not use plastic, plastic coated or embossed cards).
  • Page 101: Pal Auto Sampler

    Fit the end of the plunger into its holder and secure it by closing the latch mechanism. Replace the cover plate and tighten the knurled knob. Reconnect all cables and tubing and turn on the mains power to the SavantAA and GF5000. GBC SavantAA Operation Manual...
  • Page 102: Syringe Trouble-Shooting

    If air bubbles appear, check for any leaks and tighten the syringe if necessary. Then repeat the above procedure until all bubbles are removed. Replace the cover plate and tighten the knurled knob. GBC SavantAA Operation Manual...

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