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Basic information

contrAA 600

Edition 01/2014

WARNING! OPTICAL RADIATION!

NOTE

This symbol must be observed to obtain correct measurement results.

The manual uses the following system:



The numbering of the chapters and figures is consecutive.



Each figure has its own caption.



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]

Содержание contrAA 600

Страница 1: ...contrAA 600 HR CS Atomic Absorption Spectrometer Operating manual...

Страница 2: ...rademark 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 Documentation numb...

Страница 3: ...p 36 6 1 Supply and control connections 36 6 2 Setting up the contrAA 600 37 6 3 Installation and start of the ASpect CS program 38 6 4 Graphite tube technique 39 6 4 1 Connections in the sample chamb...

Страница 4: ...and bar for supply and control connections on the right side of the contrAA 600 36 Fig 18 Bar for supply and control connections 37 Fig 19 Rear view of the contrAA 600 with connections for the supply...

Страница 5: ...weights of the components of the contrAA 600 19 Table 2 Gases in the graphite tube technique 21 Table 3 Exhaust unit requirements 21 Table 4 Use and sample volume of different graphite tube variation...

Страница 6: ...t CS control software based on the Windows operating system assumes the complete instrument control of the base instrument and the accessories as well as data recording and evaluation The determinatio...

Страница 7: ...ses the following system The numbering of the chapters and figures is consecutive Each figure has its own caption Instructions for actions which occur in chronological order are numbered and com bined...

Страница 8: ...he use of this device e g work protection regulations accident prevention regulations safety regulations References to potential dangers in the manual do not replace the work protection regulations wh...

Страница 9: ...ly authorized technicians Only Analytik Jena service engineers or specially trained electrical staff may open any com ponents of the instrument especially the xenon lamp housing CAUTION SHORT CIRCUIT...

Страница 10: ...absorbent material such as cotton wool laboratory wiping cloths or cellulose The affected areas are then to be wiped with an Incidin Plus solution For cleaning the interior of the contrAA 600 the ope...

Страница 11: ...er location CAUTION HIGH TEMPERATURES During graphite tube furnace operation high temperatures occur Observe the required cooling times Do not touch the hot components during or directly after a measu...

Страница 12: ...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 SENSITIVE ELECTRONICS Always electrical...

Страница 13: ...Safety instructions contrAA 600 Edition 01 2014 11 2 2 Warning signs on the contrAA 600 Observe the warning signs on the device The following warning signs are displayed on the contrAA 600...

Страница 14: ...Emission of UV radiation Danger of short circuit Handling with jewelry not allowed 2 Warning sign next to mains switch Read operating manual before switching on the device 3 Warning sign on the back o...

Страница 15: ...focal spot in hot spot mode automatic hot spot tracking simultaneous drift correction Lamp current 9 16 A 8 A stand by operation Mode DC monitoring of burning duration and ignition impulses Power supp...

Страница 16: ...ace fuse Type Protected circuit TR5 T 100 mA 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 aut...

Страница 17: ...between room temperature and 3000 C in steps of 1 C Temperature time programming furnace program Up to 20 steps can be freely programmed within determined limits 0 to 999 s step in intervals of 1 s T...

Страница 18: ...ent Mass 7 2 kg Cooling Maintenance free cooling system for the heat dissipation of Xe lamp and graphite furnace according to the water air heat exchanger principle integrated into the spectrometer Ac...

Страница 19: ...atibility The contrAA 600 has been tested for radio interference elimination and interference immuni ty and fulfills the requirements stipulated by DIN EN 61326 Environmental compatibility The contrAA...

Страница 20: ...e requirement Environmental conditions Supply with inert gas and additive gas Exhaust unit Mains connection CAUTION OBSERVE THE SAFETY INSTRUCTIONS Observe the safety instructions in chapter Safety in...

Страница 21: ...h mm Height mm Depth mm Weight kg On the work table contrAA 600 785 653 765 974 160 AS GF 250 550 380 7 2 AS F 340 350 460 6 5 AS FD Autosampler Fluidik module 340 360 350 310 460 165 6 5 3 5 HS 60 mo...

Страница 22: ...es Switch on conditions Voltage 200 220 240 V 10 factory adjustable voltage may differ in accordance with terms of delivery Frequency 50 60 Hz or different if specified in conditions and terms of supp...

Страница 23: ...Jena AG Recommended inert gas Inlet pressure Consumption Recommended for graphite tube operation Argon 4 8 or superior Permitted components Oxygen 3 ppm Nitrogen 10 ppm Hydrocarbons 0 5 ppm Humidity 5...

Страница 24: ...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 are hung i...

Страница 25: ...Installation conditions contrAA 600 Edition 01 2014 23 Fig 3 Dimensions of the contrAA 600 top view Fig 4 Installation layout of the contrAA 600...

Страница 26: ...fic radiation source of the traditional AAS hollow cath ode lamp HCL is replaced by a single continuum source for all elements and lines a Xenon short arc lamp The special electrode geometry of the Xe...

Страница 27: ...romator based on a prism and an Echelle grating monochromator This results in a very compact design paired with a very high spectral resolution high spectral decomposition of the radiation of 145 000...

Страница 28: ...pectra The result is a simultaneous double beam system with just a single optical path which results in much higher measurement stability compared to the traditional LS AAS The sensitivity comparable...

Страница 29: ...ture ratios along the entire tube length Realization of linear temperature time runs according to a sensorless control model on the basis of saved thermoelectrical parameters and an adaptive control P...

Страница 30: ...located The trans versely heated graphite tube is pneumatically pushed against the graphite electrodes via its contact surfaces There is another graphite component located between the metal bodies th...

Страница 31: ...tube and is also directed outside through the funnel insert in the dosing opening The outer gas flow is responsible for ensuring that the graphite tube is surrounded by inert gas even when the inner...

Страница 32: ...Graphite tube variations furnace parts and inserts Standard graphite tube Graphite tube for solid analysis Graphite tube with PIN platform 1 Graphite tube standard 2 Graphite tube for solid analysis...

Страница 33: ...ide the graphite tube on a semiconductor receiver Using two wavelengths for detection a quotient signal is derived for temperature measurement which is independent of the degree of radiation of the gr...

Страница 34: ...diluent Fig 14 Autosampler AS GF The autosampler AS GF accepts defined volumes of different solutions and places them into the graphite tube It enables the Addition of up to five modifiers to the samp...

Страница 35: ...unted with the solid sample into the graphite tube The solid autosampler SSA 600 enables automatic transport of solid samples into the graphite tube furnace Weighing is performed fully automatically w...

Страница 36: ...e available 139 positions Sample tray with 129 sample positions for 15 mL Sarstedt cups on the outer track and 10 sample positions for 50 mL Sarstedt cups on the inner track 54 positions Sample tray w...

Страница 37: ...the mixing cup by first placing the concentrate into the mixing cup Then the diluent is added at a high dosing speed max volume V 25 mL A fixed waiting time ensures complete mixing A second dia phrag...

Страница 38: ...the contrAA 600 please ensure that the user instructions de scribed in Chapter Installation conditions p 18 are always complied with If the con trAA 600 has to be moved please follow the instructions...

Страница 39: ...le adapter 5 Fuses F3 F4 6 Fuses F1 F2 encapsuled 7 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...

Страница 40: ...tion Check the cooling water level p 59 6 Establish the electrical connection for the contrAA 600 Section Energy supply p 19 7 Connect the PC and the contrAA 600 with USB cable 3 in Fig 18 8 Further w...

Страница 41: ...ctrodes 5 Fuse at the graphite tube furnace 6 Illumination for furnace camera 7 Radiation sensor Fig 20 Graphite tube atomizer in sample chamber 1 Cooling water hoses red 2 7 Gas connections for inert...

Страница 42: ...justed by the manufacturer The connections for gas and cooling water are firmly installed on the graphite tube furnace The cooling water container is located under the furnace behind the cover 6 4 2 S...

Страница 43: ...e the IC graphite tube with the PIN platform 6 4 3 Inserting the graphite tube into the graphite tube furnace Removing and installing a graphite tube is necessary after the atomization method has been...

Страница 44: ...ters of the inserted graph ite tube to 0 7 Format the graphite tube In the Tube area click the Formation button Section Formatting the graphite tube p 43 Fig 25 Graphite tube furnace opened with inser...

Страница 45: ...tube temperature in the remaining four stages is measured The corrected furnace tem perature ensures correct measurement results At a formatting factor of 10 an automatic temperature correction no lo...

Страница 46: ...of electrical plug in contacts may occur NOTE Choose a safe location for the completion of the AS GF 1 Switch off the contrAA 600 before installing the AS GF 2 Install the tube guide 5 in Fig 26 to t...

Страница 47: ...uspension of the autosampler must be moved forward or back To this end unhook the autosampler from the sample chamber Move the left and right suspension mounts with the aid of adjusting screw 1 and th...

Страница 48: ...be used during graphite operation for this purpose 13 Switch off the AAS device and install the hydride system e g HS 60 modular 14 For the HydrEA technique remove the tube guide and dosing tube from...

Страница 49: ...he furnace Adjustment of the dipping depth Carry out the following work steps successively Withdraw the dosing tube approx 8 mm from the canula of the autosampler and fix it with a clamp nut Replace t...

Страница 50: ...hnical autosampler parameters 6 5 3 Populating the sample tray of the AS GF 1 Populate the positions of the AS GF as follows Positions 1 100 1 5 mL sample cups Positions 101 108 5 mL special cups 2 Pl...

Страница 51: ...entric back up rolls must be premounted for hanging the solid autosampler SSA 600 so that they can still be rotated 1 In the sample chamber screw the holding pin onto the left AS GF support and loosel...

Страница 52: ...60 modular and the autosampler are placed on a separate table in front of the contrAA 600 Fig 31 HydrEA system HS 60 modular Work steps Installation 1 Switch off the contrAA 600 2 Install the HS 60 m...

Страница 53: ...ent marking 1 through the tube guide at the autosampler arm and plug it onto the thicker canula of the autosampler arm 10 Set the sample tray on the autosampler housing make sure it clicks into place...

Страница 54: ...ond tube end to the valve 2 in Fig 33 4 Screw the dosing tube for the diluent encased marking 1 to the second connection of the valve 3 in Fig 33 5 Immerse the hose for the wash liquid marking 2 into...

Страница 55: ...the AAS device is switched off 1 On the PC close the application program ASpect CS Click the File Exit menu options 2 For unsaved values decide whether unsaved data information should be saved before...

Страница 56: ...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 su...

Страница 57: ...a clear pressure loss is detected by the manometer Mobile cooling unit for xenon lamp and graphite tube furnace Stabilization vessel Check the filling level in the stabilization vessel If neces sary f...

Страница 58: ...witched on when the contrAA 600 is reactivated and initialized Protection from uncontrolled furnace heating A second safety circuit protects the AAS in the event of a possible communication error betw...

Страница 59: ...uses CAUTION CONTAMINATION OF THE LAMP WINDOW Do not touch the lamp window when exchanging the lamp Decontaminations have a nega tive impact on the lamp properties 1 Open the lamp chamber door at the...

Страница 60: ...ing water hoses to the bottom of the lamp housing Press the plug connectors of the hoses into their counterparts at the lamp housing left hose left inlet right hose right inlet and push them in as far...

Страница 61: ...lled 7 4 Check the cooling water level Check the cooling water level monthly The container for the cooling liquid for cooling the graphite tube furnace and xenon lamp is located under the graphite tub...

Страница 62: ...jacket ceramic ring and graphite tube can be the cause of substandard analysis results CAUTION THERE IS A RISK OF BURNING YOURSELF ON THE HOT GRAPHITE TUBE FURNACE Allow the graphite tube furnace to...

Страница 63: ...urnace windows exhibit brittleness and cracks replace the sealing rings Fig 38 Identical markings at the furnace windows facing upward 7 5 2 Cleaning the graphite surfaces The graphite surfaces must b...

Страница 64: ...The graphite tube should be replaced Work steps see Chapter Inserting the graphite tube into the graphite tube furnace p 41 7 5 4 Replacing the electrodes and the furnace jacket If the electrodes hav...

Страница 65: ...spanner and unscrew it completely by hand Caution Risk of breaking the insulating ring Do not jam the face spanner 7 Screw the press out tool into the movable furnace part with the spindle turned back...

Страница 66: ...ng tool small bracket 13 Use the ratchet wrench to insert the elec trode to the stop Loosen the inserting tool and remove it Caution Risk of breaking the electrode Make sure that the electrode and the...

Страница 67: ...ectors for the inner gas flow into the furnace jacket on both sides Attach the two other gas tubes to the corre sponding gas connectors 19 Screw in the covering screw at the rear of the fixed furnace...

Страница 68: ...ner 24 Check visually that the insulating ring protrudes approx 0 3 mm from the jaw 25 Attach the furnace window to the furnace jacket and insert the pipetter insert 26 Insert the knurled pin arrow to...

Страница 69: ...the dosing tube is not immersed properly into the wash cup during washing the autosampler must be realigned in the wash position 4 In the window Function tests enable the button Adjust autosampler In...

Страница 70: ...unction tests in the ASpect CS software 7 6 2 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 w...

Страница 71: ...rAA 600 and start the ASpect CS software 3 In ASpect CS open the window Autosampler with Change to the tab Function tests Fig 40 p 68 4 In the area Tracker Rotator enter 101 into the list field and en...

Страница 72: ...o 15 3 Push the dosing tube as far as possible into the tube guide until the dosing tube pro trudes by approx 8 mm at the bottom 4 Lock the dosing tube with the clamp nut 5 Readjust the injection dept...

Страница 73: ...ston of the dosing syringe moves down 5 Unscrew the fixing screw 3 in Fig 42 6 Unscrew and remove the dosing syringe 2 in Fig 42 7 Screw the new dosing syringe to the valve 8 Carefully pull the piston...

Страница 74: ...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 auto matically drained of...

Страница 75: ...change over valve 6 Screw the new tube set with dosing tube marking 1 to the change over valve and attach the encased tubes with the attachment lug to the rear of the autosampler 7 Insert the tube wi...

Страница 76: ...0 p 13 In addition it is not possible to get an adequate grip for transport without the screw in handles There is a risk of injury if transport is attempted without using the handles or by too few peo...

Страница 77: ...ons must be neutralized for example with a diluted sodium hydroxide solution The neutralized waste must be brought to the appropriate waste disposal center for correct disposal according to the approp...

Страница 78: ...ce of A 0 0044 corresponds to 1 absorption analog characteristic concentration Formatting Heating the graphite tube furnace via several predefined tempera ture set points to the maximum temperature Th...

Страница 79: ...lution which originates after treating the sample to be analyzed according to the analysis instructions If no additional processing steps are required this is the measuring solution Pyrolysis Most eff...

Страница 80: ...l 61 Cooling water pump 60 D Dosing tube cleaning 71 replacing 72 shortening 72 E Electrode 33 cleaning 63 Electrodes replacement 64 Emergency shut down 8 F Format 45 Furnace camera 33 Furnace jacket...

Страница 81: ...p detector 27 monochromator 27 Solid sampler installation 51 Solid samplers types 35 Switch off the contrAA 600 55 T Technical data graphite tube furnace 16 instrument fuses 15 optical system 14 PC 16...

Страница 82: ...EC Declaration of Conformity 80 Edition 01 2014 contrAA 600 12 EC Declaration of Conformity...

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