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Summary of Contents for Analytik Jena contrAA 600
- Page 1 600 HR-CS Atomic Absorption Spectrometer Operating manual...
- Page 2 Copyrights and Trademarks contrAA is a trademark of Analytik Jena AG registered in Germany. Microsoft, Windows 7/8, MS Excel are registered trademarks of Microsoft Corp. The identification with ® or TM is omitted in this manual.
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Page 3: Table Of Contents
Graphite tube technique ......39 General safety instructions ......6 6.4.1 Connections in the sample chamber for the Warning signs on the contrAA 600 ....11 graphite tube technique ....... 39 Specification..........13 6.4.2 Software presets for the graphite tube Technical data .......... - Page 4 Fig. 2 Dimensions of the contrAA 600 - front view22 Fig. 23"Main Settings" window for graphite tube Fig. 3 Dimensions of the contrAA 600 - top view 23 technique ..........40 Fig. 4 Installation layout of the contrAA 600 ..23 Fig.
- Page 5 List of tables Table 1 Measurements and weights of the Table 5 Furnace parts and inserts ......31 components of the contrAA 600 ....19 Table 6 Maintenance overview ......55 Table 2 Gases in the graphite tube technique ..21 Table 7 Fuses ............
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Page 6: Basic Information
HydrEA technique. It is used for the sequential trace detection of metals and non-metals in liquid and dissolved samples. Combined with an autosampler the contrAA 600 can be used as a multi element automat in routine analysis. First, the elements of interest are calibrated. For this purpose, the calibra- tion standards and then also the samples are processed sequentially. - Page 7 Instructions for actions which occur in chronological order are numbered and com- bined in action units. Menu and option sequences in the software are divided by "/" and are printed in bold, e.g. File / Open. Buttons are marked with square brackets, e.g. [OK]. contrAA 600 Edition 01/2014...
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Page 8: Safety Instructions
Safety instructions Safety instructions For your own safety and to ensure error-free and safe operation of the contrAA 600, please read this section carefully before using the appliance. Comply with all safety instructions in the manual and pay careful attention to all messages and notes which are displayed on the screen by the control software. - Page 9 Safety instructions INSTRUMENT SHUTDOWN IN CASE OF DANGER! In an emergency, switch off the contrAA 600 using the power switch right side wall. Discon- nect the mains plug from the mains socket. Switch off the installed components using the mains switch of the connected socket strip.
- Page 10 This list is in so far incomplete that other solvents could also come into consideration for use in the contrAA 600 in the HydrEA technique. In cases of uncertainty about an un-named fluid, this may only be used when the manufacturer has confirmed that there is no danger to safety.
- Page 11 MAINTENANCE Service, maintenance and repair work on the contrAA 600 may only be carried out by service engineers from Analytik Jena AG or by technicians authorized by the manufacturer. Excep- tions to this are described in Section "Care and maintenance" p. 54. If these requirements are not complied with, there is a serious risk of misalignment or damage to the device.
- Page 12 Only use replacement parts from Analytik Jena AG. The graphite tubes of the contrAA 600 are manufactured specifically and may only be or- dered from Analytik Jena AG. Do not use any other graphite tubes. The contrAA 600 may be damaged.
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Page 13: Warning Signs On The Contraa 600
Safety instructions Warning signs on the contrAA 600 Observe the warning signs on the device! The following warning signs are displayed on the contrAA 600: contrAA 600 Edition 01/2014... -
Page 14: Fig. 1 Warning Signs On The Contraa 600
Warning sign next to mains switch (Read operating manual before switching on the device!) Warning sign on the back of the contrAA 600 (Disconnect AC line before removing cover!) Warning sign on the mains fuse cover (Warning! Disconnect AC line before removing cover. Changing mains fuses only by authorized personnel.) -
Page 15: Specification
Specification Specification Technical data 3.1.1 Data on contrAA 600 Optical system Reflexion optics with protective coating and optical system with light-proof enclosure Monochromator Echelle, grating, double monochromator with a focal length of F=380 mm and variable intermediate gap; upstream monochromator with quartz prism. Wavelength selection via... - Page 16 Graphite tube furnace Power supply fuse The power supply fuses may only be changed by service engineers from Analytik Jena AG or by technical personnel author- ized by Analytik Jena AG. gL-G instrument fuse fittings (10×38 mm²) according to 60947-3.
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Page 17: Control Computer Data
43 cm color monitor (17") VGA graphic card Resolution 800x600 pixels or higher, CD ROM Ports: 2 x USB interface (USB 1.1 or 2.0) for the contrAA 600 Mouse, printer Printer Inkjet printer HP DeskJet Laser printer HP Laser Jet... -
Page 18: Data For Hydrea Technique 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 Edition 01/2014 contrAA 600... -
Page 19: Guidelines And Standards
DIN ISO 9022-2:2003/01 EC directives The contrAA 600 is built and tested according to standards that fulfill the requirements stipulated by the EC directives 2006/95/EC and 2004/108/EC. Each device leaves the manu- facturer in a pristine and technically safe state. To maintain this condition and to ensure safe operation, the operator must strictly observe the safety and operating instructions contained in this manual. -
Page 20: Installation Conditions
Danger from toxic and chemically aggressive substances Environmental conditions Do not set up the contrAA 600 directly beside a door or a window. The work space of the contrAA 600 should be free of draft, dust, corrosive vapor and also vibrations. ... -
Page 21: Space Requirement And Weight
The contrAA 600 is operated on single-phase alternating current. The current load can reach 85 A for a short period (1 s) during maximum heating. The mains voltage at the contrAA 600 should not decrease by more than 6 % during this period. For any deviation from these values, please contact Analytik Jena AG. -
Page 22: Gas Supply
The mains connection shall be protected on the input (building) side with a 35 A slow-blow fuse and must be installed prior to delivery of the contrAA 600 near the assembly point. The instrument cable is 3 m long. The CEE surface socket (2 pole + E blue 5UR 3 206-2 220/32, Siemens) is supplied according to the terms of deliv- ery. -
Page 23: Exhaust Unit
Exhaust unit SWITCH ON THE EXHAUST UNIT DURING OPERATION! Do not operate the contrAA 600 without an exhaust unit! Direct waste air to atmosphere and avoid blockages! The exhaust unit should remove any ozone. Ozone is caused by the reaction of air and UV radiation from the xenon lamp and the graphite tube furnace. -
Page 24: Device Layout And Space Requirement
This prevents interference with the integrated cooling system on the left of the contrAA 600. The PC and the printer can also be placed on a regular PC table. The accessories for the graphite tube technique – autosampler AS-GF for dissolved samples or solid sampler SSA 6 or SSA 600 for solid samples –... -
Page 25: Fig. 3 Dimensions Of The Contraa 600 - Top View
Installation conditions Fig. 3 Dimensions of the contrAA 600 - top view Fig. 4 Installation layout of the contrAA 600 contrAA 600 Edition 01/2014... -
Page 26: Functions And Setup Of The Contraa 60024
In addition, absorption lines and absorption bands of diatom- ic molecules (PO, CS,...) may be used for analytic element determination. Atomizer The following atomization techniques are displayed on the contrAA 600: Graphite tube technique for liquid samples ... -
Page 27: Fig. 6 Beam Path In The Contraa 600
2100 °C or 800 °C respectively. Finally, the contrAA 600 with its graphite tube technique is also suitable for the direct solids analysis in connection with the special sample periphery SSA 600. With the determination of trace elements directly in the solid sample, the time-intensive and contamination-prone sample digestion can be eliminated as the main source of error in solution analysis. -
Page 28: Xenon Lamp
LS AAS is achieved when using 3 to 5 measurement pixels per absorption profile. The extremely low-noise CCD line receiver in the contrAA 600 allows a signal-to-noise-ratio that is, to some extent, considerably improved compared to the photomultipliers that are normally used with the LS AAS and thus present much better detection and determination limits. -
Page 29: Electrothermal Atomizer
Fig. 8 Electrothermal atomizer – graphite tube furnace The electrothermal atomizer [EA] is an integral part of the contrAA 600 and the core piece for working in EA mode and the HydrEA technique. The furnace system is equipped with a graphite tube, which has contact pieces at the side of the tube jacket for a transversely aligned pipe heater. -
Page 30: Graphite Tube Furnace
Functions and setup of the contrAA 600 Thermal pretreatment, separating (ashing or pyrolysis of) distorting sample incidental substances (matrix) Atomizing the sample Cleaning the graphite tube and preparing for the next measurement. The operator optimizes these basic steps for each analysis problem with the ASpect CS control software. -
Page 31: Gas Flows In The Graphite Tube Furnace
Functions and setup of the contrAA 600 5.3.2 Gas flows in the graphite tube furnace The furnace jacket houses the gas channels for the separate supply of the inner gas flow (purge gas) and the outer gas flow (protective gas). Oxidizing or reducing gases (O or H can be added to the inner gas flow if necessary. -
Page 32: Graphite Tube Variations, Furnace Parts And Inserts
Functions and setup of the contrAA 600 1, 4 Cylinder for furnace windows 2, 3 Holder: Cone attachment Fig. 11 Graphite tube furnace When changing from the normal tube to the platform tube or to the solid analysis, bear in mind that the platform tube covers the free opening for the beam passage on one side. -
Page 33: Radiation Sensor
Functions and setup of the contrAA 600 Fig. 13 Furnace jacket, adapters and inserts Furnace part / insert Function Platform (sample carrier) Accommodates solids samples. Adjusting aid for SSA 600 Adjusts the solid autosampler SSA 600. Pipetter insert Funnel opening to the pipetting channel. -
Page 34: Accessories For The Graphite Tube Technique
Functions and setup of the contrAA 600 Accessories for the graphite tube technique 5.4.1 Autosampler AS-GF The autosampler AS-GF is used in the EA mode for feeding the liquid samples and in the HydrEA technique for feeding the reaction gas into the graphite tube. -
Page 35: Solid Sampler Ssa 600 And Ssa 6Z
Functions and setup of the contrAA 600 The AS-GF is hung in the adapters provided in the sample chamber and electrically con- nected to the contrAA 600. The device parameters of the AS-GF are set with the ASpect CS control software. -
Page 36: Supplementary Accessories
More information on the Hg/hydride systems can be found in the relevant accessory manu- als. 5.5.2 Autosampler AS-F and AS-FD for HydrEA technique The following autosamplers can be used for the HydrEA technique with the contrAA 600: the autosampler AS-F ... -
Page 37: Fig. 16 Autosampler As-Fd With Separate Fluidik Module
Fluidik module is electrically connected to the autosampler and is supplied with operating voltage via the contrAA 600. Standards or samples are diluted in the mixing cup by first placing the concentrate into the mixing cup. Then the diluent is added at a high dosing speed (max. -
Page 38: Installation And Start-Up
The supply lines are connected during the assembly of the contrAA 600 by service engineers from Analytik Jena AG. The mains switch is located on the right side of the contrAA 600. The right side also has easily accessible connections for PC and accessories. The media connections for gas and electricity as well as the fuses are located at the rear. -
Page 39: Setting Up The Contraa 600
Fuses F1, F2 (encapsuled) Main connection line for contrAA 600 Fig. 19 Rear view of the contrAA 600 with connections for the supply of gas and electrici- ty as well as the fuse holders Setting up the contrAA 600 CAUTION! ONLY SERVICE ENGINEERS ARE ALLOWED TO INSTALL... -
Page 40: Installation And Start Of The Aspect Cs Program
Check the cooling water and refill if necessary (→ Section "Check the cooling water level" p. 59). Establish the electrical connection for the contrAA 600 (→ Section "Energy supply" p. 19). Connect the PC and the contrAA 600 with USB cable (3 in Fig. 18). Further work steps: − Install ASpect CS software −... -
Page 41: Graphite Tube Technique
Dosing opening with graphite funnel insert Gas connections for inert and protective gas, black Graphite tube Furnace jacket Movable furnace part Fixed furnace part Ceramic ring Power cable Fig. 21 Connections at the graphite tube furnace contrAA 600 Edition 01/2014... -
Page 42: Software Presets For The Graphite Tube Technique
Set the options for the graphite tube technique in the Main Settings window of the Aspect CS software. The software interface with the method and device parameters is adjusted accordingly. Fig. 23"Main Settings" window for graphite tube technique Edition 01/2014 contrAA 600... -
Page 43: Inserting The Graphite Tube Into The Graphite Tube Furnace
Inserting the graphite tube into the graphite tube furnace In ASpect CS use to open the Furnace window. Go to the Control tab. Fig. 24 "Furnace / control" window Open the graphite tube furnace with the [Open furnace] button. contrAA 600 Edition 01/2014... -
Page 44: Graphite Tube Furnace Opened With Inserted Graphite Tube
Open the graphite tube furnace with the [Open furnace] button in the Furnace / Con- trol window (Fig. 24 p. 41). Remove the graphite tube with plastic tweezers, or by hand protected with cellulose wadding. Insert the new graphite tube (see above) and/or close the graphite tube furnace. Edition 01/2014 contrAA 600... -
Page 45: Formatting The Graphite Tube
Ramp [°C/s] Heating rate Hold [s] Set the hold time Start the cleanout with the [Start] button in the furnace area. Cleaning may be repeated several times, if required at a higher temperature. contrAA 600 Edition 01/2014... -
Page 46: Complete And Install The As-Gf Autosampler44
Installing the AS-GF CAUTION! ELECTRONICS MAY BE DAMAGED! Switch off the contrAA 600 before installing the AS-GF! The electronics of the contrAA 600 are very sensitive. Damage due to connection or discon- nection of electrical plug-in contacts may occur. NOTE Choose a safe location for the completion of the AS-GF. -
Page 47: Installing The As-Gf
Place and fix the sample tray on the axis of the AS-GF. Place the sample cover until it sits in the guide rail. 10. Switch on the computer and the contrAA 600, wait for the initialization steps to com- plete, start the ASpect CS software. -
Page 48: Adjusting The As-Gf
The AS-GF has already been installed according to Section "Installing the AS-GF" p. 44. The fine alignment of the AS-GF to the furnace is supported by software. The autosampler is aligned such that samples can be optimally deposited in the graphite tube. Edition 01/2014 contrAA 600... -
Page 49: As-Gf Adjustment
Adjust the Z direction software-controlled: Lower the autosampler arm up to the upper edge of the adjusting aid until the dos- ing tube just dips into the dosing opening. Adjustments for X and Z direction are saved in the software. contrAA 600 Edition 01/2014... -
Page 50: Populating The Sample Tray Of The As-Gf
The population of the sample tray must match the software configuration in the method or in the sample ID. 6.5.4 Uninstalling the autosampler AS-GF Switch off the contrAA 600! For HydrEA coupling: Remove the reaction gas tube from the titan canula. Remove the titan canula from the autosampler arm, by loosening the clamp nut. -
Page 51: Notes On Installing The Automatic Solid Autosampler Ssa 600
SSA 600 CAUTION! ELECTRONICS MAY BE DAMAGED! Switch off the contrAA 600 before installing the SSA 600! The electronics of the contrAA 600 are very sensitive. Damage due to connection or discon- nection of electrical plug-in contacts may occur. CAUTION! -
Page 52: Installations For Hydrea Operation
Plug the control cable into the socket of the autosampler (rear) and fasten. Place the autosampler AS-FD (with Fluidik module) next to the HS 60 modular. Plug the control cable into the "AS" socket on the right side wall of the contrAA 600 (7 in Fig. 18 p. 37) and fasten. -
Page 53: Rear Of The Autosampler As-Fd
12. Position the sample cover in such a way that the guiding spout of the autosampler casing takes hold of the groove of the lid. 13. Switch on the contrAA 600 and start the software. Fluidik module connection AAS connection... -
Page 54: Starting Up The Contraa 600 With Accessories52
Switch on the PC and wait for the computer program to initialize: The application icons appear on the screen, including the ASpect CS program icon. Switch on the contrAA 600: Press the green ON/OFF switch on the right side wall. Start the ASpect CS program: Double-click with the mouse cursor on the ASpect CS icon. - Page 55 ASpect CS is exited after a 30 s delay. Shut down the PC. Use the respective mains switches to switch off (in this order): − − − Printer The AAS system is now switched off. contrAA 600 Edition 01/2014...
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Page 56: Care And Maintenance
The contrAA 600 must be switched off before carrying out any service work, the mains plug must be pulled out. The safe disconnection of the contrAA 600 from the mains can only be achieved by pulling out the mains plug. Power is still supplied to certain areas of the spec- trometer, as well as the output socket, after the device has been switched off at the main switch. -
Page 57: Base Device
Switch off the contrAA 600 and pull the mains plug from the 35 A connection before replac- ing fuses! The fuses of the contrAA 600 are on the back of the device, at the connection strip and the sample chamber of the graphite tube furnace. They are marked. -
Page 58: Reactivating The Safety Circuits Of The Cooling Water Circuit
65°C. Damage to the device that would be caused if the furnace is still heating can be avoided. If the second safety circuit has switched off the power supply, the error message "Timeout autosampler" appears when the contrAA 600 with graphite tube technique is reactivated. -
Page 59: Cleaning The Sample Chamber
Removing and installing the xenon lamp WARNING! ELECTRIC SHOCK! Switch off the contrAA 600 at the mains switch. It is very important that you also remove the mains plug from the 35 A connection before replacing fuses! CAUTION! CONTAMINATION OF THE LAMP WINDOW! - Page 60 Note: There should be an audible click when the hoses are plugged in and the interlock in the connection piece of the lamp housing should pop out. Switch on the contrAA 600. 10. Make sure that circulation pump works and cooling water flows back to the stabilization vessel.
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Page 61: Check The Cooling Water Level
Sensor for level monitor Cover Cooling water container Fig. 37 Cooling water container under the graphite tube furnace Unscrew the attachment screws of the cover plate (2 in Fig. 22, p.40) and remove the cover plate. contrAA 600 Edition 01/2014... -
Page 62: Maintaining The Graphite Tube Furnace
After cleaning the sample chamber window with alcohol, it takes approx. 1 h until the com- plete UV transmission has been restored. Only use cleaning solution for cleaning (order no. 407-320.002). Preparation of the cleaning solution: Use a mixture of demineralized water and 1 vol% clean- ing solution. Edition 01/2014 contrAA 600... -
Page 63: Cleaning The Graphite Surfaces
Cleaning the graphite surfaces The graphite surfaces must be cleaned after daily use as required. Switch on the contrAA 600 and start the ASpect CS software (the movable furnace part must be pressurized to be opened/closed). In ASpect CS use to open the Furnace window. -
Page 64: Cleaning And Changing The Graphite Tube
Face spanner Ratchet wrench Fig. 39 Furnace tools Switch on the contrAA 600 and start the ASpect CS software (the movable furnace part must be pressurized to be opened/closed). In ASpect CS use to open the Furnace / Control window. - Page 65 Unscrew the press-out tool from the furnace part completely. Pull the furnace window off of the furnace jacket and remove the pipetter insert. contrAA 600 Edition 01/2014...
- Page 66 Caution! Risk of breaking the furnace jacket! When inserting, always make sure that the furnace jacket and the fixed furnace part are in parallel. If the furnace jacket has un- Edition 01/2014 contrAA 600...
- Page 67 (small bracket). Insert the electrode to the stop into the jaw using the ratchet wrench. Caution! Do not tilt the electrode. It may break! 22. Any graphite dust should be removed by suction or blown away. contrAA 600 Edition 01/2014...
- Page 68 The connecting rod must be in the front po- sition. 27. Screw the covering screw to the movable furnace part. 28. Close the furnace with the [Close furnace] button. Edition 01/2014 contrAA 600...
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Page 69: Autosampler As-Gf
Switch on the contrAA 600 and start the ASpect CS software. In ASpect CS open the window Autosampler with Use the [Wash] button to start the wash cycle. -
Page 70: Servicing The Dosing Tube
A defective or kinked dosing tube or one with sediment deposits can be the cause of distort- ed measurement results. Maintenance work is: Cleaning the dosing tube Shorten the dosing tube Replace the dosing tube Edition 01/2014 contrAA 600... -
Page 71: Dosing Tube At The As-Gf
Fill the sodium hypochlorite solution into a 5 mL special cup and mount tray position 101 with it. Switch on the contrAA 600 and start the ASpect CS software. In ASpect CS open the window Autosampler with . Change to the tab Function tests (Fig. - Page 72 Screw the new dosing tube to the valve and feed it through the tube holders. Push the dosing tube into the tube guide until it protrudes 8 mm at the bottom, lock with the clamp nut. Readjust the injection depth of the sample (→ section "Adjusting the AS-GF" p. 46). Edition 01/2014 contrAA 600...
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Page 73: Replacing The Metering Syringe
Fig. 42 Dosing unit at AS-GF and AS-FD Switch on the contrAA 600 and start the ASpect CS software. In the window Main Settings Select technique: Graphite furnace (AS-GF) or Flame (AS-FD). to open the Autosampler window. Change to the tab Function tests. -
Page 74: Automatic Samplers As-F, As-Fd
Loosen the fixing screw on the autosampler arm. Pull the canula guide with canulas upwards and out. Fit the guide with the new canulas into the autosampler arm and fix in place with the locking screw. Edition 01/2014 contrAA 600... -
Page 75: Replacing The Intake Tube
Autosampler window. Change to the tab Function tests. In the area Pumps enable the checkbox Mix cup pump to start the pump. Run the pump until the liquid has been drained off. Disable the checkbox Mix cup pump, to stop the pump. contrAA 600 Edition 01/2014... -
Page 76: Transporting The Contraa 600
(included in scope of supply). The contrAA 600 is too heavy for two persons (→ Section "Data on contrAA 600" p. 13). In addition, it is not possible to get an adequate grip for transport without the screw-in handles. -
Page 77: Waste Disposal
The neutralized waste must be brought to the appropriate waste disposal center for correct disposal according to the appropriate legal guidelines. At the end of its service life, the contrAA 600 and all its electronic components must be disposed of as electronic waste in accordance with valid regulations. -
Page 78: Abbreviations / Terms
Identity and weight. Identity data and weight/mass of a sample. Continuum source Radiator, the radiation of which is continually distributed over a large wavelength range. The contrAA 600 uses a xenon lamp as an excitation source. Neutral value solution Solution which contains the chemicals used for creating the sample solution and also the components which influence the measurement in the same or similar concentration as the sample to be analyzed. - Page 79 The stock solution is used for making reference solutions. Background compen- Evaluation of measurement value with no background. The back- sation ground compensation occurs simultaneously. Background meas- Measurement of the spectral background in the environment or urement under the analysis line. contrAA 600 Edition 01/2014...
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Page 80: Index
30 gas flows 31 Connection maintenance 62 AS-GF 46 device 38 graphite tube furnace 41 contrAA 600 High Resolution Continuum Source (HR-CS) activation 54 installation 39 measuring principle 26 switch off in case of danger 8 Monochromator 27 transport preparation 77... - Page 81 / function test 69 monochromator 27 Furnace / Control 43 Solid sampler Main Settings 42 installation 51 Solid samplers types 35 Xenon lamp 28 Switch off the contrAA 600 55 cooling 55 exchange 59 function 26 contrAA 600 Edition 01/2014...
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Page 82: Ec Declaration Of Conformity
EC Declaration of Conformity EC Declaration of Conformity Edition 01/2014 contrAA 600...
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