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Analytic Jena contrAA 300 Operating Manual

High-resolution continuum source atomic absorption spectrometer
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contrAA 300
High-Resolution Continuum Source
Atomic Absorption Spectrometer
Operating manual

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Summary of Contents for Analytic Jena contrAA 300

  • Page 1 300 High-Resolution Continuum Source Atomic Absorption Spectrometer Operating manual...
  • Page 2 Service: Analytik Jena AG Customer Services Konrad-Zuse-Str. 1 07745 Jena Germany Phone: Hotline: + 49 (0) 3641 / 77-7407 77-7449 Fax: + 49 (0) 3641 / Email: service@analytik-jena.de General information about Analytik Jena AG on the internet: http://www.analytik-jena.de Copyrights and Trademarks contrAA is a registered trademark of Analytik Jena AG in Germany.

  • Page 3: Table Of Contents

    Energy supply ..................17 Gases used in flame mode ..............17 Laboratory fume hood .................18 System layout & general view .............19 Functions and design of the contrAA 300 ....21 Basic unit .....................21 5.1.1 Physical measuring principle of HR-CS AAS ..........21 5.1.2...
  • Page 4 Change of burner head .................. 45 6.3.6 Installing the scraper at a later stage.............. 45 6.3.7 Operation of the HPT burner head ..............46 Start-up of contrAA 300 with accessories ...........47 6.4.1 Turn-on sequence, daily start of work ............47 6.4.2 Shutdown sequence ..................47 Care and maintenance ..........

  • Page 5: Basic Information

    The contrAA 300 Atomic Absorption Spectrometer is a PC-controlled device for the sequential trace analysis of metals and non-metals in liquid and dissolved samples. The contrAA 300 is a flame device providing the possibility to use the hydride technique in combination with the Hydride System (HS) accessory.
  • Page 6 Besides, they can be used as a basis for user-defined multielement analysis methods. The control software contains comprehensive presentation and storage options for measured signals and parameters, GLP-compliant result records and various options for quality control including the possibility of keeping quality control cards. Issue 01/2014 contrAA 300...

  • Page 7: Safety Instructions

    Device switch-off in emergency situations! Switch off the contrAA 300 with the power switch on the right side panel. Disconnect the power cable from the power outlet. Switch off installed system components with the power switch of the connected multiple socket outlet, which should be placed in a way to allow fast access.
  • Page 8 Be careful if acetylene is escaping! Acetylene is an explosive gas that is easily detected by its smell. Shut down the contrAA 300 if gas paths are leaking and fuel gas valves or safety devices of the automatic gas control system are defective.
  • Page 9 Keep combustible materials away from the device. Ventilation Take care to ensure that the ventilation systems on the contrAA 300 and the accessory units are always functional. Covered vents, ventilation slots, etc. may result in malfunction or damage to the device.
  • Page 10 Ensure that the flame sensor is always functional. If gas paths are leaking, or if detect a fault on the fuel gas valves or the safety devices of the automatic gas control system, switch off the contrAA 300 until the fault has been remedied.

  • Page 11: Specifications

    Specifications Technical data Specifications Technical data 3.1.1 contrAA 300 Optical system Reflecting optics with protective coating and optical system in light-proof casing Monochromator Optimized high-resolution Echelle double monochromator. Pre- monochromator with quartz prism. Wavelength accuracy ensured through automatic neon wavelength correction Wavelength range 185 –...
  • Page 12 Max. 90 % at +30 °C Storage temperature –40 °C to +50 °C acc. to DIN 58390-2 (desiccant) Dimensions and weights Weight 90 kg Dimensions (W x H x D): 890 mm × 450 (540) mm × 545 mm Issue 01/2014 contrAA 300...

  • Page 13: Control Computer

    Resolution 800x600 Pixel or higher , CD ROM Ports: – Mouse port – Printer port - USB port (USB 1.1 or 2.0) for contrAA 300 Printer HP DeskJet Ink Jet Printer HP Laser Jet Laser Printer Operating system Windows XP Professional 3.1.3...

  • Page 14: Accessories

    Sample tray 139/ 15 Sample cups 129 pieces, 15 mL Special cups 10 pieces, 50 mL Sample tray 54/ 50 Sample cups 54 pieces, 50 mL Power supply Via AAS basic instrument Wash bottle Mass 6.5 kg Issue 01/2014 contrAA 300...
  • Page 15 Sample volume for single analysis 300 µL (minimum volume) Power supply Via spectrometer Piston Compressor JUN-AIR 6/S Standard Tank capacity 15 L Dimensions (diameter × height) 400 mm × 480 mm Power supply 230 V, 50 Hz Weight 28 kg contrAA 300 Issue 01/2014...

  • Page 16: Guidelines And Standards

    DIN EN 61010-1 (VDE 0411T.1; IEC 1010-1) • DIN EN 61010-2-061 (IEC 1010-2-061) • Electromagnetic Compatibility (EMC) The contrAA 300 has been tested for radio interference suppression and noise immunity. It complies with the requirements of DIN EN 61326 • EC Directives...

  • Page 17: Installation Requirements

    300. The operator of the device is responsible everything not included in the scope of delivery of the contrAA 300, but needed for its operation. The operation of the contrAA 300 necessitates that certain technical requirements be met: Suitable installation site •...

  • Page 18: Floor Space Requirements And Weight

    Floor space requirements and weight You are advised to prepare samples and store wet-chemical materials in • a separate room. In the operating room of the contrAA 300, smoking is not allowed. • Operating temperature range: +10 °C to 35 °C •...

  • Page 19: Energy Supply

    Do not use an adapter in the mains supply line. Do not use any automatic circuit breakers. The contrAA 300, PC, monitor and printer are to be connected to a power outlet via a common multiple socket outlet and thus to the same phase. To avoid abrupt voltage fluctuations, do not connect the contrAA 300 to a circuit, to which other high energy consuming equipment has been connected.

  • Page 20: Laboratory Fume Hood

    Gases for flame technique Laboratory fume hood Laboratory fume hood Do not operate the contrAA 300 without fume hood! Direct waste gas to the outside and avoid blockage! The laboratory fume hood shall exhaust noxious combustion residues of the flame and any produced ozone. Ozone is produced by the interaction of air and the UV radiation emitted by the xenon lamp and the burner flame.

  • Page 21: System Layout & General View

    For placement of accessory items for Hg/hydride technique (HS 60 A, HS 60), an extra table on the left-hand side in front of the contrAA 300 is used. Located on the floor in a position directly beside the product are these components: •...
  • Page 22 Installation requirements System layout & general view Fig. 4-2 Top-side dimensional view of contrAA 300 Fig. 4-3 Layout view of contrAA 300 Issue 01/2014 contrAA 300...

  • Page 23: Functions And Design Of The Contraa 300

    Functions and design of the contrAA 300 Basic unit Functions and design of the contrAA 300 Basic unit 5.1.1 Physical measuring principle of HR-CS AAS The measuring principle of both High Resolution Continuum Source Atomic Absorption Spectrometry (HR-CS AAS) and classical Line Source AAS (LS AAS) is based on the absorption of primary radiation by the analyte atoms in their ground state.
  • Page 24 Functions and design of the contrAA 300 Basic unit lines or bands of diatomic molecules (PO, CS, ...) can be used analytically for element determination. Atomizer Like in classical LS AAS, the atomizer used for the flame technique is a burner- nebulizer system with a pneumatically aspirating nebulizer.

  • Page 25: Xenon Lamp

    These are achieved by the use of the CCD line detector of the contrAA 300 with extremely low noise compared to the photomultipliers customary in LS AAS and to the use of the high-energy xenon short-arc lamp with its very high light intensity.

  • Page 26: Flame System

    Functions and design of the contrAA 300 Basic unit 5.1.3 Flame system Flame atomic absorption spectroscopy is used for the determination of trace elements in the concentration range from mg/L to µg/L and for the determination of principal components. The technique requires a flame with constant properties.
  • Page 27 Functions and design of the contrAA 300 Basic unit The sample aerosol hits the impact bead, where larger droplets condense and then drain away through the siphon. The fuel gas flow hits the impact bead at right angles. Once generated, the aerosol flows through the mixing chamber to the burner.
  • Page 28 Functions and design of the contrAA 300 Basic unit Combustion gas supply Siphon Baffle ball Outflow from siphon Nebulizer Float switch Sample liquid supply Impeller Oxidant supply 10 Mixing chamber tube Fig. 5-4 Nebulizer-mixing chamber-burner system The setup of the mixing chamber nebulizer system optimizes the aerosol formation and ensures that the system is easy to maintain.
  • Page 29 Functions and design of the contrAA 300 Basic unit readjustment after cleaning the mixing chamber nebulizer system is not required. Burner Fixing screw for siphon Fixing screw for burner 10 Siphon Combustion gas supply 11 Connection of siphon sensor Additional oxidant supply...
  • Page 30 Functions and design of the contrAA 300 Basic unit 5.1.3.3 Burner and flame type The contrAA 300 can be operated with the following types of flames and corresponding burners: Acetylene/air flame with 50-mm single-slot burner (standard burner) or • 100-mm single-slot burner (sensitivity increases by a factor of 1.5 – 1.8...

  • Page 31: Accessories For Flame Technique

    The parameters are set and the function is controlled with the contrAA 300 control software. The contrAA 300 P can be operated with the following autosamplers: The autosampler AS-F is an automatic autosampler.
  • Page 32 The autosampler AS-FD features an extra Fluidik module with a dosing unit (5000 µL). The Fluidik module is electrically connected to the autosampler and is supplied with operating voltage via the contrAA 300. Standards or samples are diluted in the mixing cup by first placing the concentrate into the mixing cup.

  • Page 33: Jun-Air 6/S Piston Compressor

    Functions and design of the contrAA 300 Accessories for flame technique 5.2.2 JUN-AIR 6/S Piston Compressor If no in-house compressed-air supply is available, it is useful to use a compressor that produces the air required for the acetylene/air flame. The JUN-AIR 6/S Piston Compressor is available as option. The produced compressed air is free from water, dust and oil.

  • Page 34: Scraper - Automatic Burner Head Cleaner For Nitrous Oxide Flame

    Functions and design of the contrAA 300 Accessories for flame technique 5.2.4 Scraper – Automatic burner head cleaner for nitrous oxide flame The Scraper, an intelligent burner head cleaner, is recommended for the continuous and fully automated operation with the nitrous oxide flame. When...

  • Page 35: Supplementary Accessories - Hg/Hydride Systems

    Functions and design of the contrAA 300 Supplementary accessories – Hg/hydride systems The quartz glass has a slit with a length of 50 mm on opposite sides to allow the flame to pass through. The holder ensures that the slits are aligned to the burner head.

  • Page 36: Installation And Start-Up

    AAS measurement environment. Always observe all warning and information labels affixed to the device or displayed by the contrAA 300 control software. To ensure trouble-free operation of the contrAA 300 take care to always keep the ambient conditions specified in Section "Installation requirements"...
  • Page 37 PC USB/B port PC COM port Fuses for xenon lamp Fig.6-2 Power supply and control connector strip Connector strip Air connector fuel connector Type label O nitrous oxide connector Fig.6-3 Rear view of contrAA 300 with supply connectors contrAA 300 Issue 01/2014...
  • Page 38 SFS 6 and scraper 15 Fixing screw for holder bracket of burner- Vertical adjustment of burner-nebulizer nebulizer system unit system unit Fig. 6-4 Terminals at the burner-nebulizer system unit available for flame technique Issue 01/2014 contrAA 300...

  • Page 39: Installation And Start Of Aspect Cs Software

    Terminal facilities provided in sample compartment walls Installation and start of ASpect CS software Installation and start of the ASpect CS software required for the control of the spectrometer are described in the ASpect CS user manual. contrAA 300 Issue 01/2014...

  • Page 40: Flame Technique

    Burner Sample container Holder bracket at vertical adjustment Sample tablet Collector trough mechanism Siphon drain tube Mixing-chamber-nebulizer system unit Gas terminals Supply cable of siphon sensor Sample aspiration tube Fig. 6-6 Flame technique, manual sample delivery Issue 01/2014 contrAA 300...
  • Page 41 11. Attach the aspiration tube to the nebulizer canula. 12. Hang the safety glass in and slide it in front of the burner. 13. Switch on the contrAA 300 and start the software. Working steps for deinstallation 1. Turn the contrAA 300 off.

  • Page 42: Installation For Continuous Operation Mode / Sample Supply By Autosampler

    Flame mode, continuous with autosamplers AS-FD and SFS 6 Installing the burner/nebulizer system 1. Switch off the contrAA 300. 2. Remove the red protective cap from the mixing chamber tube. 3. Attach the mixing chamber nebulizer system without burner to the holding fixture for the height adjustment.
  • Page 43 4. Plug the control cable into "Sampler flame" connection on the right-hand wall of the contrAA 300 (4 in p. Fig.6-2 p. 35) and lock it in place. 5. Attach the outlet tube to the outlet connector of the autosampler (backplate, 4 in Fig.
  • Page 44 11. Place the sample cover until it sits in the guide rail. Fluidik module connection AAS connection Suspension mount with adjusting screw Connector for outlet tube Screw for wash tube Fig. 6-8 Rear of the autosampler AS-FD Issue 01/2014 contrAA 300...

  • Page 45: Uninstalling The Autosampler As-F/As-Fd

    5. Immerse the hose for the wash liquid (marking "2") into the storage bottle. 6.3.3 Uninstalling the autosampler AS-F/AS-FD 6. Switch off the contrAA 300. Uninstalling the autosampler 7. Detach the sample intake tube from the thin canula of the autosampler arm.

  • Page 46: Installation Of The Sfs 6 Injection Module

    Tube connecting to rinsing solution Fig. 6-10 SFS 6 installed at the contrAA 300 for manual sample delivery 1. Screw aspiration tubes into free ports of the injection module as follows: screw short tube piece into middle port – linking up with the nebulizer screw long tube piece into uppermost port –...

  • Page 47: Change Of Burner Head

    2. Unscrew the fastening rail (1 in Fig. 6-12) with knurled screws (3 in Fig. 6-12) from the scraper. The captive knurled screws remain attached in their holder in the scraper. contrAA 300 Issue 01/2014...

  • Page 48: Operation Of The Hpt Burner Head

    2. Set the HPT burner head on the connector of the mixing chamber and clamp. 3. Set a burner height of 12 mm or more for flame ignition and operation. Issue 01/2014 contrAA 300...

  • Page 49: Start-Up Of Contraa 300 With Accessories

    ASpect CS software. 2. Switching on the contrAA 300: Actuate the green ON/OFF switch on the right side panel. 3. Start ASpect CS software by a double click on the ASpect CS icon.
  • Page 50 Installation and start-up Start-up of contrAA 300 with accessories 1. On the PC in ASpect CS software: Activate menu function File / Exit Application. (If this menu is not accessible, refer to the ASpect CS manual for alternatives.) 6. If there is any data/information that has not yet been saved, decide whether you want to save it before exiting the ASpect CS application.

  • Page 51: Care And Maintenance

    In maintenance work, observe all guidelines, standards and safety instructions specified in Section "Safety instructions" p. 5. To ensure perfect and safe functioning of the contrAA 300, it should be inspected on an annual basis by service technicians from Analytik Jena AG.

  • Page 52: Basic Device

    7.2.1 Fuse change Make sure to switch off the contrAA 300 before changing any fuses! The fuses of contrAA 300 are located at the connector strip of the device (see Fig.6-3). The fuses are labeled with their numbers. Fuse Number...

  • Page 53: Cleaning The Sample Compartment

    • Removing and installing the continuum source (Xe lamp) Warning! Electric shock hazard! Switch off the contrAA 300 with the power switch and disconnect it from the power outlet before changing the lamp! Contamination of lamp windows! Take care not to touch the lamp window surfaces! Any contamination will impair...
  • Page 54 Note: When pushing in the plug couplings, a click sound must be heard and the locks in the connectors of the lamp housing jump out. 9. Switch on the contrAA 300. 10. Verify that the recirculation pump is working and cooling water flowing back into the compensating vessel.

  • Page 55: Burner-Nebulizer System

    Crusts formed in the burner slot in the analysis of solutions having high • salt contents cannot be removed with the cleaning rod. Burn hazard! Allow the burner to cool down before servicing it. Procedure 1. Disassemble the burner-nebulizer system. 2. Clean the burner. contrAA 300 Issue 01/2014...

  • Page 56: Disassemble Burner-Nebulizer System Unit

    Mixing chamber screw joints (4 x) Safety plug Locking ring for nebulizer 10 Knurled head screw on the holding bow Fixing screw for siphon Connection of siphon sensor Fig. 7-3 Deinstalling and taking the burner-nebulizer system unit apart Issue 01/2014 contrAA 300...
  • Page 57 (8 in Fig. 7-3) and pull off the tube from the nebulizer connector. 3. Turn the locking ring of the nebulizer (4 in Fig. 7-3) to open the locking. Withdraw the nebulizer from the mixing chamber head, holding the contrAA 300 Issue 01/2014...

  • Page 58: Clean Burner

    Caution: The spacers must not protrude over the upper side of the burner jaws (arrow Fig.7-8 p. 58)! When using a scraper, it remains attached. 6. Screw the burner jaws onto the burner body, the dowel pins (4 in Fig. 7-6) on the burner ensure correct positioning. Issue 01/2014 contrAA 300...
  • Page 59 1;3 Burner jaw fittings against each other Fittings of the burner jaws with the burner body Dowel pins on the underside of the burner jaws Fig. 7-6 Fittings of the burner Burner jaw Burner jaw Spacers Burner body Fig.7-7 Burner, disassembled contrAA 300 Issue 01/2014...

  • Page 60: Clean Nebulizer

    1. Clean with saltpeter, diluted mineral acid, or the appropriate solvent according to the substances analyzed. Clean the channels with a round brush. 2. If the siphon is cleaned with a diluted mineral acid, wash thoroughly with distilled water after cleaning. 3. Wash the float holder. Issue 01/2014 contrAA 300...

  • Page 61: Assemble Burner-Nebulizer System Unit

    (beam passage of xenon lamp). 4. Open the Manual Optimization tab. 5. Let the nebulizer draw in test solution, for example, Cu / 2 mg/L, then trigger continuous display mode of measured values. Evaluate the signal. contrAA 300 Issue 01/2014...

  • Page 62: Cleaning The Sensor Of The Burner

    (10 in Fig. 7-3). 2. Clean the sensor cautiously with the help of a little brush, for example a toothbrush, using alcohol, for example Isopropanol. 3. Reinstall the burner-nebulizer-system on the holding bow. Fig. 7-10 Sensor of the burner Issue 01/2014 contrAA 300...

  • Page 63: As-F, As-Fd Autosampler

    3. Use the [Start] button to start the wash cycle. 4. The wash cycle can be repeated several times if required. 25 mL of washing liquid is dispensed from the storage bottle into the mixing cup and automatically drained off afterwards. contrAA 300 Issue 01/2014...

  • Page 64: Replacing The Canulas And Guide On The Autosampler Arm

    3. Insert the new canula and fix with the clamp nut. Caution! Risk of fracture! Set the canula height for it to terminate 1-2 mm above the washing cup. 4. Plug the intake tube onto the new canula. Issue 01/2014 contrAA 300...

  • Page 65: Replacing The Intake Tube

    8. Screw the tube for the washing liquid to the rear of the autosampler. 9. Slide the other end of the dosing tube through the tube guide onto the thicker canula of the autosampler arm. contrAA 300 Issue 01/2014...

  • Page 66: Replacing The Dosing Syringe

    Drive rod Fig. 7-11 Dosing unit at AS-FD 1. Switch on the contrAA 300 and start the ASpect CS software. In the window Main Settings Select technique: Flame. 2. Use to open the Autosampler window. Change to the tab Function tests.

  • Page 67: Compressor Jun-Air 6/S

    Allow air to escape from time to time by turning the knurled nut. The valve position is thus prevented from sticking and the functioning is guaranteed. Note: Do not damage the seal and do not alter the setting of the safety valve! contrAA 300 Issue 01/2014...

  • Page 68: Relocating The Contraa 300

    2. Close the door of the sample compartment. 3. Shut off the gas supply at the gas mains. 4. Disconnect the gas supply tubes on the back panel of the contrAA 300: Use the 19-mm open-end wrench for the acetylene connector.

  • Page 69: Setting Up The Contraa 300

    Tighten acetylene connector by means of the 19-mm open-end wrench. Caution: Left-hand thread! 4. Check whether gas connectors are leak-proof (see Section "Supply and control connections", p. 34). 5. Establish electrical connections to the contrAA 300. contrAA 300 Issue 01/2014...

  • Page 70: Disposal

    The neutralized waste must be disposed of properly in compliance with the relevant statutory provisions. At the end of its service life, the contrAA 300 and all its electronic components must be disposed of as electronic scrap in accordance with valid regulations.

  • Page 71: Ec Declaration Of Conformity

    EC Declaration of Conformity Setting up the contrAA 300 EC Declaration of Conformity contrAA 300 Issue 01/2014...

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