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Analytik Jena multi EA 4000 Operating Manual

Elementary analyzer c, s and cl solids analysis
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Elementary analyzer
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Operating manual

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Summary of Contents for Analytik Jena multi EA 4000

  • Page 1 EA 4000 Elementary analyzer C, S and Cl solids analysis Operating manual...
  • Page 2 Copyrights and Trademarks multi EA and multiWin are registered trademarks of Analytik Jena AG in Germany. Microsoft, Windows, MS Excel are registered trademarks of Microsoft Corp. The identification with ® or TM is omitted in this manual.

  • Page 3: Table Of Contents

    Automatic TIC solids module....................33 4.5.1 Technical data ........................33 4.5.2 Layout ..........................34 Manual TIC solids module ....................38 4.6.1 Technical data ........................38 4.6.2 Layout of the manual TIC solids module ................39 multi EA 4000 Version 01.16...
  • Page 4 Operation ........................51 Switching on / heat-up phase / setup ..................51 C/S measurement ......................... 52 7.2.1 Preparing the multi EA 4000 and C/S module ..............52 7.2.2 Performing the C/S measurement ..................55 Carbon detection after pyrolysis ................... 57 7.3.1 Preparing the multi EA 4000 and C/S module ..............
  • Page 5 Prepare the manual TIC solids module and analyzer ............80 7.6.2 Performing the TIC measurement ..................80 Maintenance and care ................... 84 Basic device multi EA 4000 ....................84 8.1.1 Clean and maintain the device ..................... 84 8.1.2 Check the hose connections ....................84 Operation with C/S module ....................
  • Page 6 Installing the multi EA 4000 C/S ..................122 10.3.2 Installing the multi EA 4000 Cl .................... 125 10.3.3 Installing the multi EA 4000 C/S Cl ..................127 10.3.4 Installing the automatic TIC solids module................131 10.3.5 Installing the manual TIC module ..................134 10.4...
  • Page 7 Status indicators at the basic device multi EA 4000 ............. 24 Fig. 6 Control elements behind the front doors of the multi EA 4000 ..........25 Fig. 7 Connections on the right-hand side of the multi EA 4000 ............ 25 Fig.
  • Page 8 Hose diagram multi EA C/S with manual TIC solids module ..........135 Fig. 43 Hose diagram multi EA C/S Cl with manual TIC solids module .......... 136 Fig. 44 Retrofit kit for FPG 48 to use the boat storage ..............142 Edition 01/2016 multi EA 4000...

  • Page 9: Basic Information

    Buttons are marked with square brackets, e.g. [S Intended Use The elementary analyzer multi EA 4000 is a device for the detection of the total carbon con- tent and/or total sulfur content or for the detection of the total chlorine content in solid and paste-like samples.

  • Page 10: Warranty And Liability

    Due to the many specific configuration options the multi EA 4000 is suitable for use in teach- ing and research. The analyzer multi EA 4000 must only be used for the methods for the detection of total car- bon and/or total sulfur content or the detection of the total chlorine content in solid, paste-like or liquid samples described in this user manual.

  • Page 11: Technical Data

    Technical data Technical data General characteristics Designation/type Analyzer multi EA 4000 Dimensions Basic device (W x H x D) 550 x 500 x 550 mm per module: 300 x 500 x 550 mm Sampler: 520 x 500 x 700 mm Mass approx.
  • Page 12 1000 °C Heat-up period up to 30 min. Analysis time up to 10 min. – dependent on the combustion time and concentration Sample weight Up to 3000 mg (dependent on consistency and matrix) Edition 01/2016 multi EA 4000...

  • Page 13: Safety Instructions

    Indicates a potentially hazardous situation. If it is not prevented light or minor injuries and material damage can result. CAUTION! HOT SURFACE! Touching the hot surface can cause burns. WARNING! DANGER OF ELECTRIC SHOCK IF TOUCHED! multi EA 4000 Version 01.16...

  • Page 14: Safety Markings On The Analyzer

    Any changes in the analyzer affecting its safety must be reported by the operating personnel to the operator without delay.  The equipment components must only be connected to supply cables intended and designed for this purpose. Edition 01/2016 multi EA 4000...

  • Page 15: Requirements For The Operating Personnel

    Requirements for the operating personnel The analyzer multi EA 4000 must only be operated by qualified specialist personnel instruct- ed in the use of the analyzer. The instruction must also include conveying the content of this user manual and the user manuals of other system components or add-on equipment.

  • Page 16: Safety Instructions - Operation

     The ventilation equipment on the multi EA 4000 and the extension modules must be in good working condition. Covered vents or ventilation slits etc. may cause the de- vice to break down or may cause damage to it.

  • Page 17: Safety Instructions - Protection Against Explosion And Fire

     Any work on the right-hand side component of the analyzer may only be carried out by the customer service of Analytik Jena AG and specially authorized technicians.  The electrical components must be checked regularly by a qualified electrician. Any defects, such as loose connections, faulty or damaged cables, must be repaired without delay.

  • Page 18: Handling Of Auxiliary And Operating Materials

    When handling the above-mentioned concentrated acids, observe in particular the following notes:  The concentrated acid can cause burns and irritation!  Always wear goggles and protective gloves when handling concentrated acids!  Ensure adequate ventilation in the laboratory rooms. Edition 01/2016 multi EA 4000...
  • Page 19 Methanol must not enter the sewage system, surface water or ground water! The applicable regulations for disposal must be meticulously observed.  Only store the methanol well sealed in its original container! Observe the notes on the labels. multi EA 4000 Version 01.16...
  • Page 20 Thymol must not enter the sewage system, surface water or ground water! The ap- plicable regulations for disposal must be meticulously observed.  Only store thymol sealed in its original container! Observe the notes on the labels. Edition 01/2016 multi EA 4000...
  • Page 21 (titration cell) or in the module housing. Acetic acid vapor is not only corrosive but also hazardous to health. Do not inhale these vapors! Always connect the adsorption tube with active carbon in the chlorine module without delay! multi EA 4000 Version 01.16...

  • Page 22: Safety Instructions - Service And Repair

    3.7.6 Safety instructions - service and repair The analyzer is usually serviced by the customer service department of Analytik Jena AG or its authorized and trained specialist personnel. Independent servicing can maladjust or damaged the analyzer. Therefore, the operator may generally only carry out the tasks listed in chapter 'Maintenance and care' p.

  • Page 23: System Design

    System design System design Comprehensive overview The analyzer multi EA 4000 is of modular design. The basic device (combustion unit) is combined with one or several detector modules dependent on the task:  Basic device  Carbon and/or sulfur module (C/S module) ...

  • Page 24: Pneumatic And Hose System

    Horizontal furnace Open gas airlock Fig. 1 Horizontal furnace of the basic device multi EA 4000 4.2.2 Pneumatic and hose system Hose system The connection between the individual components and to the analysis modules is made via a hose system.

  • Page 25: Components For Measuring Gas Drying And Cleaning

    " flow meter for intake flow "pump" Fig. 2 Flow meters at the basic device multi EA 4000 4.2.3 Components for measuring gas drying and cleaning Dust trap for C/S detection The dust trap is attached directly to the ceramic combustion tube. Combustion dust settles inside it.

  • Page 26: Indicator And Control Elements, Connections

    The green LED at the left door of the analyzer illuminates after the analyzer has been switched on. Fig. 5 Status indicators at the basic device multi EA 4000 Behind the front doors there are the mains switch and the flow meters for the manual control of the gas flows.

  • Page 27: Fig. 6 Control Elements Behind The Front Doors Of The Multi Ea 4000

    Connections on the right-hand side of the multi EA 4000 On the rear of the multi EA 4000 are the gas inlets for the oxygen and argon supply, the connections for the attachment to the C/S or Cl module and the mains connection cable.

  • Page 28: C/S Module

    "Ar" for argon during Cl measure- ments and pyrolysis "out" connection – measuring output Fig. 8 Connections on the rear of the multi EA 4000 C/S module C/S module versions The C/S detector module is available in three versions: ...

  • Page 29: Fig. 9 Indictors And Connections At The C/S Module

    Deviations from the permissible target value are indicated, and the intake flow can be cor- rected at the "pump" valve of the flow meter of the basic device multi EA 4000 (3 in Fig. 6). During a measurement the values are used for the integrated correction using the VITA method.

  • Page 30: Cl Module

    Buffer container as pressure compensation to compensate the switching pulses of the splitting valve  Adsorption tube  Halide trap The control electronics for the multi EA 4000 Cl is also located in the Cl module. adsorption tube halide trap measuring cell with electrodes stirring/cooling block Fig. 10 Cl module 4.4.1...

  • Page 31: Fig. 11 Layout Of The Measuring Cell

    Layout of the measuring cell Combination electrode The combination electrode combines the indicator electrodes (Ag), generator cathode (Pt) and gas introduction. The generator anode is a round silver blank in the two measuring cell bodies (see above). multi EA 4000 Version 01.16...

  • Page 32: Combustion Tube And Measuring Gas Drying

    The end of the combustion tube is sealed with quartz wool to prevent dust from entering the hose system of the multi EA 4000. quartz wool plug...

  • Page 33: Measuring Gas Cleaning

    The gas extracted from the measuring cell is passed via the adsorption tube. Here the acetic acid vapors escaping from the electrolyte is removed. Active carbon is used as adsorption agent. adsorption tube halide trap Fig. 15 Halide trap and adsorption tube in the Cl module multi EA 4000 Version 01.16...

  • Page 34: Connections

    The green LED located at the front of the Cl module illuminates once the module has been switched on. Dependent on the equipment of the multi EA 4000 with or without C/S module, the connec- tion for attachment to the C/S module or the basic device and the sampler are found on the rear.

  • Page 35: Automatic Tic Solids Module

    System design Automatic TIC solids module The automatic TIC solids module expands the multi EA 4000 for the detection of TIC (TC, TOC) in solids. Carbon dioxide generated by acidification and purging is passed to the NDR detector of the multi EA 4000. The following analysis modes are possible: ...

  • Page 36: Layout

    The phosphoric acid pump transports 40% phosphoric acid to the TIC reactor. Whilst the sample boat is moved continuously through the sampler FPG 48 towards the multi EA 4000, the sample is evenly diluted with phosphoric acid. Via the condensate pump the condensate is automatically pumped off after each measurement.

  • Page 37: Fig. 20 Hose Pumps At The Automatic Tic Solids Module

    C/S module. The U-tube is filled with special copper wool and brass wool. The filling of the halogen trap has to be renewed at the latest once half of the copper wool or the brass wool is discolored. multi EA 4000 Version 01.16...

  • Page 38: Fig. 21 Measuring Gas Drying And Cleaning At The Automatic Tic Solids Module

    A dust filter is located between the change-over valve on the rear of the automatic TIC solids module and the measuring gas inlet of the C/S module. Fig. 22 Dust trap before the measuring gas inlet of the C/S module Edition 01/2016 multi EA 4000...

  • Page 39: Fig. 23 Connections At The Automatic Tic Solids Module

    The connections are located on the rear of the automatic TIC solids module. mains switch connection "valve HT" for connection to the multi EA 4000 gas connection for oxygen at the TIC reactor connection "COM HT" for connection to the...

  • Page 40: Manual Tic Solids Module

    The manual TIC solids module enables the detection of TIC in solids in combination with the multi EA 4000 C or multi EA 4000 C/S. The acidification and purging of the TIC takes place at raised temperatures. The measuring gas is moved together with the carrier gas to the detector of the C/S module.

  • Page 41: Layout Of The Manual Tic Solids Module

    Flow adjustment of the carrier gas flow The carrier gas flow is adjusted via the needle valve "O2" with glass gauge on the rear of the manual TIC solids module. glass gauge needle valve Fig. 26 Flow meter for oxygen flow multi EA 4000 Version 01.16...

  • Page 42: Fig. 27 Metering Pump For Acid At The Manual Tic Solids Module

    The U-tube of the halide trap is filled with special copper wool and brass wool. The filling of the halide trap has to be re- newed at the latest once half of the copper wool or the brass wool is discolored. Edition 01/2016 multi EA 4000...

  • Page 43: Fig. 28 Components For Measuring Gas Drying And Cleaning At The Manual Tic Solids Module

    Components for measuring gas drying and cleaning at the manual TIC solids module Connections mains supply module with mains switch and fuse holder measuring gas outlet "analyte" carrier gas connection "O " Fig. 29 Connections at the manual TIC solids module multi EA 4000 Version 01.16...

  • Page 44: Other Optional Accessories

    System design Other optional accessories 4.7.1 Sampler Two sample supply versions are available for the multi EA 4000:  the solids autosampler FPG 48  the manual feed Autosampler FPG 48 The autosampler FPG 48 has space for 48 sample boats. The boats are received automati- cally by the trays and transferred to the combustion furnace.

  • Page 45: Measuring Method

    TC/TS analysis The multi EA 4000 with C/S module is a special system for the simultaneous and individual detection of total carbon and total sulfur in solid and paste-like samples through high tem- perature oxidation in the oxygen flow.

  • Page 46: Toc Analysis

    The sample digestion takes place in a TIC solids module. The measuring gas is detected in the C/S module. TOC analysis During the TOC analysis the total organic carbon content of a sample is detected. In the multi EA 4000 the TOC content can be determined in two ways:  Differential method ...

  • Page 47: Carbon Detection After Pyrolysis: Tc-Ec (Optional)

    (5) and (6) through regression calcula- tion. �� = ( �� ) /�� × �� + �� ������ �� = (�� × �� + �� × �� + �� )/�� ���������� ������ multi EA 4000 Version 01.16...

  • Page 48: Day Factor

    The multiWin software offers the option to proceed with different calibration strategies adapted to the analytical requirement and dependent on the measuring range and sample matrix. With the multi EA 4000 multi point calibrations with variable sample volumes and constant concentrations are performed.

  • Page 49: Other Calculations

      + Cl AgCl (10) From the charge volume used up for generating the silver ions the chloride volume can be calculated using Faraday's law. multi EA 4000 Version 01.16...

  • Page 50: Data Analysis In The Cl Mode

    The actual split factor is checked and, where necessary, corrected using standards. 5.7.3 Analysis The coulometric Cl detection is an absolute analysis method. No calibration is performed. The result is stated in the analysis report as absolute mass [µg] and as concentration [µg/g] or [mg/g]. Edition 01/2016 multi EA 4000...

  • Page 51: First Commissioning

    Energy supply CAUTION The analyzer multi EA 4000 must only be connected to a properly grounded mains outlet in accordance with the voltage specifications on the type plate! The multi EA 4000 is operated from the single phase alternating current mains.

  • Page 52: Gas Supply

    Unpacking and placing the analyzer IMPORTANT The analyzer multi EA 4000 must only be set up, assembled and installed by the customer service department of Analytik Jena AG or trained specialist personnel authorized by Analyt- ik Jena AG! Any unauthorized intervention in the analyzer can endanger the user and the operational safety of the equipment and limits or completely invalidates any warranty claims.

  • Page 53: Operation

    Switch on the autosampler FPG 48 (optional).  The autosampler FPG 48 initializes. Switch on the basic device multi EA 4000. Switch on the analysis module.  The devices will boot. The status lamps at the front panels of the basic device and modules illuminate.

  • Page 54: C/S Measurement

    Therefore, only switch on the analyzer with the combustion tube inserted! For conversion and maintenance activities at the combustion tube or combustion furnace, always switch off the analyzer from the mains switch and disconnect the multi EA 4000 by removing the mains plug from the mains network.
  • Page 55 (approx. 45°). With a slight rotating movement press the gas airlock against the wall holder of the multi EA 4000. The ceramic tube then slides into the receptacle of the combustion furnace. The ceramic tube is positioned correctly if...

  • Page 56: Fig. 30 Checking The Halide Trap And Drying Tube

    U tube for S detection halide trap with copper and brass wool for C detec- tion Fig. 30 Checking the halide trap and drying tube Edition 01/2016 multi EA 4000...

  • Page 57: Performing The C/S Measurement

    Operation 7.2.2 Performing the C/S measurement Switch on the basic device multi EA 4000, the C/S module and, where applicable, the FPG 48 from the main switch.  The status lamps at the device front panels illuminate. Note: If an automatic TIC solids module has been integrated, switch this on, too. This causes the longer transport path of the boat due to the intermediate TIC reactor to be taken into account.
  • Page 58 During prolonged pauses during measurement the oxygen supply can be switched off in the multiWin program saving oxygen accordingly. However the oxygen supply must be available again in time (approx. 10 min) before starting the measurement. Edition 01/2016 multi EA 4000...

  • Page 59: Carbon Detection After Pyrolysis

    EA 4000 by removing the mains plug from the mains network. For the detection of carbon after pyrolysis the multi EA 4000 must be equipped with the op- tional pyrolysis mode.
  • Page 60 The analysis system now has time for conditioning. If the intake flow differs greatly or changes subsequently, re-adjust it at the "pump" valve of the multi EA 4000. Weigh the samples on two ceramic boats each. Start the measurement by clicking on [S TART MEASUREMENT Create or select an analysis group for storing the measuring data.

  • Page 61: Cl Detection

    Therefore, only switch on the analyzer with the combustion tube inserted! For conversion and maintenance activities at the combustion tube or combustion furnace, always switch off the analyzer from the mains switch and disconnect the multi EA 4000 by removing the mains plug from the mains network.
  • Page 62  The gas airlock is fitted correctly if the gap between the contact pres- sure ring and the counter piece is approx. 1 mm wide all round. Edition 01/2016 multi EA 4000...
  • Page 63 (1). Connect the hose for the argon supply to the gas airlock (2).  The combustion tube is inserted into the multi EA 4000. Caution: The hoses must not be kinked or twisted! oxygen connection argon connection...
  • Page 64 Push the measuring gas hose (color- less) and the bypass hose (black) through the duct in the multi EA 4000. If necessary, use tweezers to pull the hoses out at the other duct end. Feed the hoses through the opening on the right-hand side of the Cl module.
  • Page 65 10. Connect the black bypass hose (9) at the top of the safety container (12). Note: For sulfuric acid containers without splitting outlet the connection hose hangs down loosely. bypass hose connection hose splitting outlet safety container multi EA 4000 Version 01.16...

  • Page 66: Preparing The Electrolyte Solution

    4 g gelatin in a beaker with 400 ml, allow to swell for 3 hours and then dissolve whilst heating to (35 – 45) °C. solution B2: dissolve 1.0 g thymol and 0.3 g thymol blue in a beaker in 500 ml methanol. solution B: Edition 01/2016 multi EA 4000...

  • Page 67: Making The Measuring Cell Available

    120 ml Place a magnetic stirring rod onto the floor of the measuring cell. Attach the measuring cell lid using the 3 knurled head screws. Place the measuring cell into the holder of the Cl module. multi EA 4000 Version 01.16...

  • Page 68: End Point Routine

    Switch on the multi EA 4000 and its device components (see section "Performing the Cl measurement" p. 67). Perform an end point routine (see section "End point routine" p. 66).

  • Page 69: Performing The Cl Measurement

    7.4.5 Performing the Cl measurement Switch on the basic device multi EA 4000, the Cl module, C/S module (only for multi EA 4000 C/S Cl) and, where applicable, the FPG 48 from the main switch.  The status lamps at the device front panels illuminate.
  • Page 70 − Click on in the sequence row to release it for analysis. All sequence rows can be released with the button  Sequence rows released for analysis have a green fill. Edition 01/2016 multi EA 4000...

  • Page 71: Checking The Splitting Ratio

    Measuring cell Standard concentration "high concentration" 1 N HCl "sensitive" 0.1 N HCl Move 50 µl of the standard on ceramic mats in a boat into the hot furnace. Using the method perform a detection: multi EA 4000 Version 01.16...

  • Page 72: Cauterizing The Quartz Boat

    C ALIBRATION 7.4.7 Cauterizing the quartz boat Quartz boats have to be cauterized  before first use  after cleaning out heavy contamination. To this end perform the measuring routine with empty quartz boats. Edition 01/2016 multi EA 4000...

  • Page 73: Tic/Toc Detection With Automatic Tic Solids Module

    Therefore, only switch on the analyzer with the combustion tube inserted! For conversion and maintenance activities at the combustion tube or combustion furnace, always switch off the analyzer from the mains switch and disconnect the multi EA 4000 by removing the mains plug from the mains network.
  • Page 74 Caution: The reactor must be centered in the holder. Move the ceramic tube into the opening of the combustion furnace and press it into the rear seal. The reactor connections must point upwards. Edition 01/2016 multi EA 4000...
  • Page 75 Secure the ceramic cannula with the red screw cap. Check that the sealing cone, seals and screw cap are fitted on the pump hose. Screw the pump hose finger-tight to the red screw cap. multi EA 4000 Version 01.16...

  • Page 76: Required Reagents

    In the acid bottle of the TIC solids module keep ortho-phosphoric acid ready. Switch on the basic device multi EA 4000, the C/S module, the automatic TIC solids module and the FPG 48 from the main switch.  The status lamps at the device front panels illuminate.
  • Page 77 The analysis system now has time for conditioning. If the intake flow differs greatly or changes subsequently, re-adjust it at the "pump" valve of the multi EA 4000. Weigh the sample on ceramic boat. Start the measurement by clicking on [S TART MEASUREMENT 10.

  • Page 78: Performing The Toc Detection In Accordance With The Differential Method Using The Automatic Tic Solids Module (Recommended Method)

    (recommended method) In the acid bottle of the TIC solids module keep 40% ortho-phosphoric acid ready. Switch on the basic device multi EA 4000, the C/S module, the automatic TIC solids module and the FPG 48 from the main switch.
  • Page 79 Operation The analysis system now has time for conditioning. If the intake flow differs greatly or changes subsequently, re-adjust it at the "pump" valve of the multi EA 4000. Weigh the sample on 2 ceramic boats. Caution: The weighted sample on boat 1 for the TIC detection must be max. 50 mg. Cover the sample with some annealed quartz sand.

  • Page 80: Toc Measurement With Direct Detection

    Perform a measurement as follows: In the acid bottle of the TIC solids module keep 10% hydrochloric acid ready. Switch on the basic device multi EA 4000, the C/S module, the automatic TIC solids module and the FPG 48 from the main switch.
  • Page 81 TIC solids module to the detector in the C/S module. − The same boat is then moved further into the furnace to detect the TOC (after re- moving the TIC) by incineration in the oxygen flow. multi EA 4000 Version 01.16...

  • Page 82: Tic Detection With The Manual Tic Solids Module

    The sample must be ground as finely as possible and homogeneous. In addition to the safety notices for the analyzer multi EA 4000 in section "Safety instruc- tions" p. 11 the following notes apply in particular to the operation of the manual solids mod-...
  • Page 83 Screw the dispenser onto the bottle. Connect the acid supply hose to the valve and the TIC head. Switch on the basic device multi EA 4000, the C/S module and the manual TIC solids module from the respective main switch.
  • Page 84 20. After completing the measurement switch off the stirring magnet and open the flask: Release the TIC head with a rotary movement. Move the tripod arm upwards, tilt it back and lock it in this position. 21. Clean and dry the flask. Edition 01/2016 multi EA 4000...
  • Page 85 (conditioning) and the dry gas flow cleans the hose system of any residual moisture. 23. Keep the heating plate at a constant temperature. Only switch off the temperature con- trol during prolonged measuring pauses. multi EA 4000 Version 01.16...

  • Page 86: Maintenance And Care

    Maintenance and care Maintenance and care of the analyzer are described in this chapter for the individual mod- ules. Observe all notices for the modules combined in your system. Basic device multi EA 4000 Maintenance intervals Maintenance task Maintenance interval...

  • Page 87: Operation With C/S Module

    (preferably overnight)! Remove the ceramic tube Arrange to have at least 75 cm of space to the right of the multi EA 4000. To do so, put aside the FPG 48 or manual feeder.

  • Page 88: Cleaning The Dust Trap

    Therefore, only switch on the analyzer with the combustion tube inserted! For conversion and maintenance activities at the combustion tube or combustion furnace, always switch off the analyzer from the mains switch and disconnect the multi EA 4000 by removing the mains plug from the mains network.
  • Page 89 10. If the ceramic tube has slid out of the airlock coupling on the right-hand side, slide it back in with a slight rotation (see section "Fit the ceramic tube to the gas airlock and insert it into the combustion furnace" p. 52). multi EA 4000 Version 01.16...

  • Page 90: Replacing The Desiccant In The Drying Tube

    Replacing the desiccant in the drying tube Drying tubes are used in the following measurement arrangements:  C/S measurement at the basic device multi EA 4000  TIC measurement in the corresponding TIC solids modules The desiccant must be replaced if visibly saturated with water If soot or other particles dis- color the desiccant, it must be replaced immediately.

  • Page 91: Replacing The Halide Trap

    8.2.4 Replacing the halide trap Halide traps are used in the following measurement arrangements:  TC measurement at the basic device multi EA 4000  Cl measurement in the Cl module  TIC measurement in the corresponding TIC solids modules...

  • Page 92: Operation With Cl Module

    (every 40 operating hours) Replace the copper and brass wool in the halide trap analog to the replacement of the halide trap in the basic device in the multi EA 4000 ( see section "Replacing the halide trap" p. 89).

  • Page 93: Servicing/Replacing The Quartz Glass Combustion Tube

    Therefore, only switch on the analyzer with the combustion tube inserted! For conversion and maintenance activities at the combustion tube or combustion furnace, always switch off the analyzer from the mains switch and disconnect the multi EA 4000 by removing the mains plug from the mains network.

  • Page 94: Servicing The Combination Electrode

    12. Fill approx. 2.5 cm quartz wool at the entrance of the quartz tube and, using a hook, push it to the tube end. 13. Then assemble the gas airlock and install the combustion tube in the furnace. Re- store all gas connections (see section "Preparing the multi EA 4000 for Cl meas- urements" p. 59). 8.3.3...
  • Page 95 Slide the measuring hose only approx. 1 cm If you slide the hose too far onto the elec- onto the electrode. This achieves gas- trode, it gets stuck on the electrode. The tightness. electrode can break when the hose is pulled out! multi EA 4000 Version 01.16...

  • Page 96: Servicing The Measuring Cells

    Seal one side of the glass tube with cotton wool and fill the adsorption agent. Seal the glass tube with cotton wool. Screw the filled adsorption tube back on finger-tight. Press the adsorption tube back into its holder. Caution: Do not twist or kink the hoses. Edition 01/2016 multi EA 4000...

  • Page 97: Operation With Automatic Tic Solids Module

    4000 ( see section "Replacing the desiccant in the drying tube" p. 88). Also replace the copper and brass wool in the halide trap analog to the replacement of the halide trap in the basic device in the multi EA 4000 ( see section "Replacing the halide trap" p. 89).
  • Page 98 13. Slide the reactor back into the coupling and secure it by tightening the knurled ring. 14. Attach the acid and gas connections to the reactor and re-install the FPG 48 (see section "Connect the reactor and sampler FPG 48" p. 73 and "Retrofitting the sam- pler " p. 142). Edition 01/2016 multi EA 4000...

  • Page 99: Cleaning The Condensation Coil

    11. Rotate the TIC solids module back into its original position. 12. Re-assemble the TIC reactor and the FPG 48 (see section "Connect the reactor and sampler FPG 48" p. 73 and "Connecting and using the sampler " p. 137). multi EA 4000 Version 01.16...

  • Page 100: Removing And Replacing The Pump Hose

    Insert the hose cartridge into the pump and allow it to engage. Screw the pump hose to the reactor. Place the acid container in the drip tray onto the TIC module. Slide the other end of the pump hose into an opening of the acid container. Edition 01/2016 multi EA 4000...
  • Page 101 Position the conveyor belt around the pump body. Press the conveyor belt upwards with one hand and rotate the bracket with the other hand to the right until it engages. 10. Push hoses 77 and 78 back onto their adapters. multi EA 4000 Version 01.16...

  • Page 102: Cleaning The Condensate Container

    Hose no. 77 (to the condensate pump) at the bottom outlet − Hose no. 74 (to the drying container) at the top outlet Slide the hoses approx. 1 cm wide onto the glass connections of the condensate container. Edition 01/2016 multi EA 4000...

  • Page 103: Operation With Manual Tic Solids Module

    4000 ( see section "Replacing the desiccant in the drying tube" p. 88). Also replace the copper and brass wool in the halide trap analog to the replacement of the halide trap in the basic device in the multi EA 4000 ( see section "Replacing the halide trap" p. 89).
  • Page 104 (disposable retention filter) must point up (arrows in Fig. on the right) Attach the large water trap to hose no. 8. Connect the small water trap to hose no. 9. Press the water traps into the clamp on the equipment backplate. Edition 01/2016 multi EA 4000...

  • Page 105: Fault Removal

    If faults cannot be remedied by the customer, the Analytik Jena AG service department must always be informed. This also applies for the repeated occurrence of individual faults. For the fault diagnosis the respective files must be sent by email to the Analytik Jena AG service department.
  • Page 106 10 s − restart operating system (PC) − switch on analyzer − start multiWin Signal echo received, check port selection Cause Remedy − incorrect interface selected check interface selection Edition 01/2016 multi EA 4000...
  • Page 107 S YSTEM COMPONENT TEST Firmware reset Cause Remedy − internal computer (firmware) has acknowledge message − restarted. initialize Firmware standby Cause Remedy − firmware was run in standby acknowledge message − initialize multi EA 4000 Version 01.16...
  • Page 108 − was detected during initialization initialize S sensor: incorrect status Cause Remedy − change to smoothing factor / repeat action LSCM switch-on failed S sensor: inactive Cause Remedy − sensor type transmission failed repeat action Edition 01/2016 multi EA 4000...
  • Page 109 Cl sensor repeat update Flow error Cause Remedy − flow state not OK. check for leaks − check gas supply pressure missing Cause Remedy − gas flow insufficient check O connection − check pressure multi EA 4000 Version 01.16...
  • Page 110 − communication fault with the basic switch basic device off/on − device initialize external furnace not present Cause Remedy − basic device not detected as hard- check connection between basic ware device and control module Edition 01/2016 multi EA 4000...

  • Page 111: Indications In The Window Device

    Module area. The following displays are possible: Display Description C-NDIR NDIR detector for carbon S-NDIR NDIR detector for sulfur Cl-AMP smallCell Chlorine module with "sensitive" cell Cl-AMP largeCell Chlorine module with "high concentration" cell multi EA 4000 Version 01.16...
  • Page 112 The temperature display shows the current furnace temperature. If the temperature display is red, the current furnace temperature does not match the temperature set in the method. In this case wait until the target temperature has been reached or check the temperature con- figuration in the method. Edition 01/2016 multi EA 4000...

  • Page 113: Equipment Fault

    With the intake pump switched on correct the intake flow at the flow meter "pump" in the basic module. − check hose system for kinked or squeezed hoses − − desiccant too wet and baked to- replace desiccant gether multi EA 4000 Version 01.16...
  • Page 114 IMPORTANT The ADU values of the NDIR detector drop slowly due to normal ageing. If the values drop within a few analyses, this indicates damage to the detector by components of the analysis gas! Edition 01/2016 multi EA 4000...

  • Page 115: Cl Module

    − coulometer – internal computer inform Service multiWin: indication error Cause Solution − − electrode connector not connected connect electrode and re-initialize device − − electrode faulty replace faulty electrode − inform Service multi EA 4000 Version 01.16...

  • Page 116: Device Communication Errors

    No connection to the autosampler Cause Solution − − no communication between basic check connection cable − device and sampler switch on sampler and initialize analyzer − sample not switched on − connection cable not connected or faulty Edition 01/2016 multi EA 4000...

  • Page 117: Analytical Problems

    (temperature depend- ence). The peak area changed due to the drift will be corrected automatically, thus the measuring results are never affected. − If the drift does not stop, inform Service. multi EA 4000 Version 01.16...

  • Page 118: Cl Detection

    "soaking" the combustion tube overnight in 10% HNO , then rinse thoroughly with distilled water and dry. Shutdown threshold below 1500 Cause Solution − − Combination electrode faulty or too Use new electrode for chlorine detection. Edition 01/2016 multi EA 4000...

  • Page 119: Tic Detection (Automatic Tic Solids Module)

    40% H is too slow. In max integration time of 600 s) this case use stronger acid (e.g. 25% HCl). Caution HCl may not be used permanently. multi EA 4000 Version 01.16...

  • Page 120: Measurements In Pyrolysis Mode (Ec)

    At temperatures above 1000 °C soot is in- high creasingly formed from organic compounds (plastics) through "coking", which is also de- tected in stage 2 as elementary carbon. The optimum furnace temperature for pyrolysis measurements is 850 °C. Edition 01/2016 multi EA 4000...

  • Page 121: Transport And Storage

    Prepare the EA 4000 and its modules for transport as follows: Basic device multi EA 4000 Switch off the analyzer from the main switch and allow the equipment to cool down. Disconnect the gas supply and unplug the mains plug from the mains outlet.

  • Page 122: Transport Notes

    Undo all connections on the back of the module. Remove the sulfuric acid container and safety container from the basic device multi EA 4000 ab. Remove the sulfuric acid container (see section "Replacing the sulfu- ric acid/cleaning the sulfuric acid container" p. 90).

  • Page 123: Storage

    The following requirements are placed on the climatic conditions in the storage room of the analyzer:  Temperature range: +5 °C to +55 °C  max. humidity: 10 % to 30 %  Air pressure: 0.7 bar to 1.06 bar multi EA 4000 Version 01.16...

  • Page 124: Recommissioning After Transport Or Storage

    Transport and storage 10.3 Recommissioning after transport or storage 10.3.1 Installing the multi EA 4000 C/S Connections For the combination of multi EA 4000 – and C/S module the following connections must have been made: multi EA 4000 connections Target  "valve"...

  • Page 125: Fig. 34 Hose Diagram For Multi Ea 4000 C/S

    Transport and storage Hose diagram Fig. 34 Hose diagram for multi EA 4000 C/S multi EA 4000 Version 01.16...

  • Page 126: Fig. 35 Hose Diagram Multi Ea C/S For Measurement In Pyrolysis Mode

    Transport and storage Fig. 35 Hose diagram multi EA C/S for measurement in pyrolysis mode Edition 01/2016 multi EA 4000...

  • Page 127: Installing The Multi Ea 4000 Cl

    Transport and storage 10.3.2 Installing the multi EA 4000 Cl Connections multi EA 4000 connections Target  "valve" Cl module "valve"  "analyte" open output  "O " Oxygen gas connection  "Ar" Argon gas connection  Mains cable Mains connection ...

  • Page 128: Fig. 36 Hose Diagram Multi Ea Cl

    Transport and storage Hose diagram Fig. 36 Hose diagram multi EA Cl Edition 01/2016 multi EA 4000...

  • Page 129: Installing The Multi Ea 4000 C/S Cl

    Transport and storage 10.3.3 Installing the multi EA 4000 C/S Cl Connections For the combination of multi EA 4000 – and C/S module - Cl module the following connec- tions must have been made: multi EA 4000 connections Target ...

  • Page 130: Fig. 37 Hose Diagram Multi Ea C/S Cl For C/S Measurements With Ceramic Tube And Oxygen Airlock

    Transport and storage Hose diagrams Fig. 37 Hose diagram multi EA C/S Cl for C/S measurements with ceramic tube and oxy- gen airlock Edition 01/2016 multi EA 4000...

  • Page 131: Fig. 38 Hose Diagram Multi Ea C/S Cl For Cl Measurements With Quartz Tube And Argon Connection

    Transport and storage Fig. 38 Hose diagram multi EA C/S Cl for Cl measurements with quartz tube and argon connection multi EA 4000 Version 01.16...

  • Page 132: Fig. 39 Hose Diagram Multi Ea C/S Cl For Measurement In Pyrolysis Mode

    Transport and storage Fig. 39 Hose diagram multi EA C/S Cl for measurement in pyrolysis mode Edition 01/2016 multi EA 4000...

  • Page 133: Installing The Automatic Tic Solids Module

    Transport and storage 10.3.4 Installing the automatic TIC solids module Connections For the combination of multi EA 4000 – and C/S module - Cl module the following connec- tions must have been made: multi EA 4000 connections Target  "valve"...

  • Page 134: Fig. 40 Hose Diagram Of The Automatic Tic Solids Module

    Transport and storage Hose diagram Fig. 40 Hose diagram of the automatic TIC solids module Edition 01/2016 multi EA 4000...

  • Page 135: Fig. 41 Hose Diagram Multi Ea C/S With Connected Automatic Tic Solids Module

    Transport and storage Fig. 41 Hose diagram multi EA C/S with connected automatic TIC solids module multi EA 4000 Version 01.16...

  • Page 136: Installing The Manual Tic Module

    Transport and storage 10.3.5 Installing the manual TIC module Make the connections For the combination of multi EA 4000 – and C/S module - TIC solids module the following connections must have been made: multi EA 4000 connections Target ...

  • Page 137: Fig. 42 Hose Diagram Multi Ea C/S With Manual Tic Solids Module

    Transport and storage Hose diagrams Fig. 42 Hose diagram multi EA C/S with manual TIC solids module multi EA 4000 Version 01.16...

  • Page 138: Fig. 43 Hose Diagram Multi Ea C/S Cl With Manual Tic Solids Module

    Transport and storage Fig. 43 Hose diagram multi EA C/S Cl with manual TIC solids module Edition 01/2016 multi EA 4000...

  • Page 139: Connecting And Using The Sampler

    Using the adjustable feet correct the height of the sampler, if necessary. The bottom edge of the opening of the gas airlock must be level with the upper edge of the storage surface of the sampler. multi EA 4000 Version 01.16...
  • Page 140 Switch on the basic device, the detector with control unit, the automatic TIC solids module, where applicable, and the FPG 48. Start the multiWin software and initialize the analyzer. Select the menu command S . A window with the same name YSTEM AMPLE GENERAL opens. Edition 01/2016 multi EA 4000...
  • Page 141 IGHER OWER lowering depth of the gripper and set the new position by clicking on [A DJUST OSITION Repeat the process until the gripper is posi- tioned just a few millimeters below the boat storage. multi EA 4000 Version 01.16...
  • Page 142 Place a boat next to the gripper and check that the boat cannot slide under the gripper. Set the new position by clicking on [ ADJUST OSITION Once the position has been adjusted click on [ SAVE AND EXIT Edition 01/2016 multi EA 4000...

  • Page 143: Filling The Sampler Fpg 48

    Do not reach into the sample rack or the boat gripper during an ongoing measurement. The FPG 48 is filled during the measurement preparation for the multi EA 4000. The multi EA 4000 and the FPG 48 must be switched on and have been initialized in the multiWin pro- gram.

  • Page 144: Retrofitting The Sampler Fpg 48 With A Boat Storage

    Fig. 44 Retrofit kit for FPG 48 to use the boat storage Unscrew the stop plate of the guide rail (1). Remove the two hexagon socket screws (2). Edition 01/2016 multi EA 4000...
  • Page 145 12. In the area place a tick for ACCESSORY MODULES EJECTION RAIL 13. Adjust the position of the gripper relative to the ejection rail (see section "Installing and adjusting the autosampler FPG 48" p. 137). multi EA 4000 Version 01.16...

  • Page 146: Using The Manual Sample Feed

    Make sure that the boat does not get wedged, otherwise correct the position of the sample feed. Using pliers remove the hot boats from the hook and place them onto the storage area to cool down. Edition 01/2016 multi EA 4000...

  • Page 147: Connecting And Using The External Scales

    EIGHT Weigh the sample on boat. Accept the value from the scales with [OK].  The weighted sample appears in the input field. Repeat steps (2) - (4) for each sequence table. multi EA 4000 Version 01.16...

  • Page 148: Disposal

    There you will receive the information regarding recycling or disposal. Analyzer At the end of its service life the multi EA 4000 and all its electronic components must be disposed of as electronic waste in accordance with the applicable regulations.

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