Endress+Hauser Analytik Jena multi EA 4000 Operating Manual
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Endress+Hauser Analytik Jena multi EA 4000 Operating Manual

Elementary analyzer c, s and cl solids analysis
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Operating Manual
multi EA 4000
Elementary analyzer
C, S and Cl solids analysis

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Summary of Contents for Endress+Hauser Analytik Jena multi EA 4000

  • Page 1 Operating Manual multi EA 4000 Elementary analyzer C, S and Cl solids analysis...
  • Page 2 Analytik Jena AG Manufacturer Konrad-Zuse-Str.1 07745 Jena  Germany Phone + 49 3641 / 77 70 + 49 3641 / 77 92 79 Email info@analytik-jena.de Analytik Jena AG Service Konrad-Zuse-Str. 1 07745 Jena  Germany Phone + 49 3641 / 77-7407 (Hotline) Email service@analytik-jena.de http://www.analytik-jena.com...

  • Page 3: Table Of Contents

    multi EA 4000 Contents Contents Basic information ......................7 User manual notes ...................... 7 Intended use ....................... 8 Warranty and liability....................9 Safety instructions ......................10 Safety markings on the analyzer ................10 Technical condition ....................11 Requirements for the operating personnel ............... 11 Safety instructions, transport and commissioning ............
  • Page 4 Contents multi EA 4000 4.7.1 End point routine ...................... 46 4.7.2 Measurement with split / split factor ................ 46 4.7.3 Analysis ........................46 Commissioning ....................... 47 Site requirements ...................... 47 5.1.1 Installation conditions....................47 5.1.2 Space requirement ....................47 5.1.3 Energy supply ......................
  • Page 5 multi EA 4000 Contents Operation with Cl module ..................114 7.3.1 Replacing the sulfuric acid/cleaning the sulfuric acid container ......114 7.3.2 Servicing/replacing the quartz glass combustion tube ..........115 7.3.3 Servicing the combined electrode ................117 7.3.4 Servicing the measuring cells .................. 118 7.3.5 Replacing the adsorption agent ................
  • Page 6 Contents multi EA 4000 Figures Figure 1 Gas sluice and horizontal furnace of the basic device multi EA 4000 ..18 Figure 2 Flow regulators at the basic device multi EA 4000 ........19 Figure 3 Dust trap at the combustion furnace............20 Figure 4 Dust filter .......................

  • Page 7: Basic Information

    multi EA 4000 Basic information Basic information User manual notes The analyzer multi EA 4000 is intended for operation by qualified specialist personnel observing this user manual. The user manual informs about the design and operation of the analyzer and provides personnel familiar with elementary analysis the necessary expertise for the safe han- dling of the equipment and its components.

  • Page 8: Intended Use

    Basic information multi EA 4000 Intended use The elementary analyzer multi EA 4000 is a device for the determination of total car- bon content and/or total sulfur content or for the determination of total chlorine con- tent in solid or paste-like samples. After appropriate sample preparation, it can also be sued for AOX determination.

  • Page 9: Warranty And Liability

    multi EA 4000 Basic information Warranty and liability The warranty duration and liability comply with the legal requirements and the provi- sions in the general terms and conditions of Analytik Jena AG. Deviations from the intended use described in this user manual result in limitations of warranty and liability in the event of a damage.

  • Page 10: Safety Instructions

    Safety instructions multi EA 4000 Safety instructions For your own safety and to ensure error-free and safe operation of the analyzer multi EA 4000, please read this chapter carefully before using the appliance. Observe all safety notes listed in this user manual and all messages and displayed by the multiWin control and analysis software on the monitor.

  • Page 11: Technical Condition

    multi EA 4000 Safety instructions Technical condition The analyzer corresponds in its design and construction to the current state of the art technology. Unauthorized modifications or changes, especially such that affect the safety of the staff and the environment, are generally not allowed. ...

  • Page 12: Safety Instructions, Transport And Commissioning

    Safety instructions multi EA 4000  The operation or servicing of the analyzer by minors or individuals under the influ- ence of alcohol, drugs or medication is not permitted.  It must be ensured that only authorized personnel works at the analyzer. ...

  • Page 13: Safety Instructions - Operation

    multi EA 4000 Safety instructions Safety instructions - operation 2.5.1 General The operator of the analyzer must make sure before each commissioning that the con- dition of the analyzers including the safety equipment is sound. This applies in particu- lar after each modification or extension of the analyzer or its repair. The following has to be observed: ...

  • Page 14: Safety Instructions - Electrical Equipment

    Safety instructions multi EA 4000 2.5.3 Safety instructions - electrical equipment Work on electrical components of the analyzer may only be carried out by a qualified electrician in accordance with the applicable electrical engineering rules. Life-threat- ening electrical voltages and high currents may occur in the interior of the analyzer! The following has to be observed: ...

  • Page 15: Handling Of Auxiliary And Operating Materials

    multi EA 4000 Safety instructions  Any leak from which gases escape (except oxygen/air) may result in an oxygen- starved atmosphere causing suffocation. The area in which compressed gas con- tainers are stored and the area around the device must be ventilated adequately to prevent the development of an oxygen-starved atmosphere.

  • Page 16: Safety Instructions: Service And Repair

    Safety instructions multi EA 4000  Auxiliary and operating materials as well as their containers may not be disposed in domestic waste or enter the sewage system or the soil. The applicable regulations for disposal of these materials must be meticulously observed. ...

  • Page 17: Function And Setup

    multi EA 4000 Function and setup Function and setup General overview The analyzer multi EA 4000 is of modular design. The basic device (combustion unit with furnace module HTS1500) is combined with one or several detector modules de- pendent on the task: ...

  • Page 18: Combustion System

    Function and setup multi EA 4000 3.2.1 Combustion system The combustion furnace is a resistor-heated horizontal furnace for combustion tem- peratures up to 1500 °C. A combustion tube serves as reactor. The carrier and combus- tion gas is supplied via an open gas sluice to the inside of the combustion tube. Be- cause the gas flow of the carrier and combustion gas is greater than the intake flow of the measuring gas, the resulting overpressure at the combustion tube inlet prevents measuring gas from escaping or ambient entering the combustion tube.

  • Page 19: Components For Measuring Gas Drying And Cleaning

    multi EA 4000 Function and setup The gas flows for carrier gas and combustion gas are controlled through manually ad- Gas flow control justable flow regulators at the front of the basic device. An integrated suction pump ensures a stable flow of the measuring gas through the detector.

  • Page 20: Figure 3 Dust Trap At The Combustion Furnace

    Function and setup multi EA 4000 Figure 3 Dust trap at the combustion furnace The dust trap is arranged easily accessible on the left side of the device behind the contact guard. Directly after the dust trap a dust filter has been installed in the gas path. It holds back Dust filter particles which the dust trap could not manage to remove from the measuring gas.

  • Page 21: Indicator And Control Elements, Connections

    multi EA 4000 Function and setup Drying tube with magnesium perchlo- rate Halide trap Figure 5 Drying tube and halide trap 3.2.4 Indicator and control elements, connections The green LED at the left door of the analyzer illuminates after the analyzer has been switched on.

  • Page 22: Figure 7 Control Elements Behind The Front Door Of The Multi Ea 4000

    Function and setup multi EA 4000 Figure 7 Control elements behind the front door of the multi EA 4000 On/Off switch Flow regulator to control the oxygen flow "O " Flow regulator to control the oxygen Flow regulator to control the "pump" intake flow or argon flow "Ar/O "...

  • Page 23: Figure 9 Connections On The Left-Hand Side Of The Multi Ea 4000

    multi EA 4000 Function and setup On the left-hand side behind the contact guard is the opening for the dust trap with Connections on the the connection for the measuring gas. left-hand side Left-hand side with dust trap contact guard Dust trap with measuring gas connection Figure 9 Connections on the left-hand side of the multi EA 4000 At the rear of the multi EA 4000 are the mains switch, the gas inlets for the oxygen...

  • Page 24: C/S Module

    Function and setup multi EA 4000 C/S module The C/S detector module is available in three versions: Versions of the C/S module  the C/S module with and SO detectors for the simultaneous determination of carbon and sulfur  the C module with detector for the determination of carbon ...

  • Page 25: Cl Module

    multi EA 4000 Function and setup Figure 11 Indications and connections at the C/S module "PC" USB port for connection to the PC Cl-Coul – connection to the Cl module "valve" connection – connection to the Gas outlet "pump" – connection to the multi EA flame sensor or automatic 4000 TIC solids module (optional)

  • Page 26: Coulometer Assembly And Measuring Cell

    Function and setup multi EA 4000 Adsorption tube Halide trap Measuring cell with electrodes Stirrer/cooling block Figure 12 Cl module 3.4.1 Coulometer assembly and measuring cell The measuring cell is available in 2 versions: "sensitive" measuring cell "high concentration" 40 ml measuring cell 150 ml Electrolyte volume approx.

  • Page 27: Figure 13 Measuring Cell Design

    multi EA 4000 Function and setup The marked opening is intended for the amperometric combined electrode. The un- marked opening is used for direct injection into the measuring cell or to connect the suction olive. When the chlorine module is switched on, the magnetic stirring rod in the measuring cell cup starts moving.

  • Page 28: Combustion Tube And Measuring Gas Drying

    Function and setup multi EA 4000 3.4.2 Combustion tube and measuring gas drying A quartz tube is used as combustion tube for Cl determination. The oxygen supply for combustion is via a bypass in the quartz tube. The measuring gas is inducted at the side connection of the quartz tube and routed via the drying to the Cl module.

  • Page 29: Measuring Gas Cleaning

    multi EA 4000 Function and setup 3.4.3 Measuring gas cleaning In the operating mode with split, the entire measuring gas from the combustion cham- Halide trap ber is divided into a defined ratio. Only some of the measuring gas reaches the meas- uring cell in order to also permit the determination of high chlorine concentrations.

  • Page 30: Figure 18 Cl Module Connections In Combination With A C/S Module

    Function and setup multi EA 4000 Figure 18 Cl module connections in combination with a C/S module Mains switch "Cl-Coul" connection – connection to the C/S module Fuse holder Gas connection "Cl" – connection to the C/S mod- mains plug connection If no C/S module has been installed, the Cl module has additional interfaces on the rear for the communication with the multi EA 4000 and the autosampler.

  • Page 31: Automatic Tic Solids Module

    multi EA 4000 Function and setup Automatic TIC solids module The automatic TIC solids module complements the multi EA 4000 for the determina- tion of the TIC (TC, TOC) in solids. Carbon dioxide generated through acidification and purging is transferred to the NDIR detector of the multi EA 4000. The following analy- sis modes are possible: ...

  • Page 32: Technical Data

    Function and setup multi EA 4000 3.5.1 Technical data General characteristics Designation/type Automatic TIC solids module Dimensions 300 x 470 x 550 mm Autosampler: 520 x 500 x 700 mm Mass approx. 5 kg Procedural data Measuring methods Detection NDIR (coupled with VITA method) Sample volume up to 3000 mg (TC) or 50 mg (TIC) Electrical variables...

  • Page 33: Figure 22 Hose Pumps At The Automatic Tic Solids Module

    multi EA 4000 Function and setup The connection between the individual components is made with labeled hoses. The Hose system hose diagram is available in section "Positioning the automatic TIC solids module" p. For the supply of the phosphoric acid and removal of the condensate, hose pumps are used.

  • Page 34: Figure 23 Measuring Gas Drying And Cleaning At The Aut. Tic Solids Module

    Function and setup multi EA 4000 Figure 23 Measuring gas drying and cleaning at the aut. TIC solids module Halide trap Drying tube Condensate container Condensation coil Peltier cooling block A dust filter has been placed between the halide trap (1 in Figure 23) and the change- over valve at the rear of the automatic TIC solids module.

  • Page 35: Figure 25 Connections At The Automatic Tic Solids Module

    multi EA 4000 Function and setup The connections are located at the rear of the automatic TIC solids module. Connections Figure 25 Connections at the automatic TIC solids module Mains switch "valve HT" connection remains empty Gas connection for oxygen at the TIC reactor "COM HT"...

  • Page 36: Manual Tic Solids Module

    Function and setup multi EA 4000 Manual TIC solids module The manual TIC solids module allows the determination of TIC in solids in conjunction with the multi EA 4000 C or the multi EA 4000 C/S. Acidification of the samples and purging of TIC is performed at elevated temperatures.

  • Page 37: Manual Tic Solids Module Setup

    multi EA 4000 Function and setup 3.6.2 Manual TIC solids module setup A 50 ml Erlenmeyer flask is used as the reactor to which a TIC head with three connec- TIC reaction chamber tions for the supply of phosphoric acid, oxygen as the carrier gas and the measuring gas outlet is attached.

  • Page 38: Figure 29 Metering Pump For Acid On The Manual Tic Solids Module

    Function and setup multi EA 4000 The acid is metered with the metering pump by hand. The hose for supplying acid to Supply of acid the reactor is connected to the metering pump with a valve. The valve in the faucet of the metering pump must be closed after acid has been supplied to the reactor.

  • Page 39: Figure 30 Measuring Gas Drying And Cleaning At The Man. Tic Solids Module

    multi EA 4000 Function and setup Drying tube Water traps Halide trap Figure 30 Measuring gas drying and cleaning at the man. TIC solids module Connections Power input module with mains switch and fuse holder Measuring gas outlet "analyte" Carrier gas connection "O "...

  • Page 40: Additional Optional Accessories

    Function and setup multi EA 4000 Additional optional accessories 3.7.1 Sampler Two versions of sampler are available for the sample feed of the multi EA 4000:  the solid autosampler FPG 48  the manual feed The autosampler FPG 48 offers space for 48 sample boats. The boats are automatically Autosampler FPG 48 picked from the trays and transferred to the combustion furnace.

  • Page 41: Measuring Methods

    multi EA 4000 Measuring methods Measuring methods The analyzer multi EA 4000 is used to determine the following parameters as sum pa- rameters.  TS – Total Sulfur  TC – Total Carbon  TCl – Total Chlorine  TOC – Total Organic Carbon ...

  • Page 42: Toc Analysis

    Measuring methods multi EA 4000 To determine the inorganic carbon (TIC), acid is added to an aliquot of the sample. This leads to the decomposition of the carbonates/hydrogen carbonates contained therein. The CO is purged and detected. No thermal oxidation takes place. 3 (CO + 2 H O + 3 CO...

  • Page 43: Direct Method For The Toc Analysis

    multi EA 4000 Measuring methods 4.3.2 Direct method for the TOC analysis With the automatic TIC solids module the TIC and TOC can also be determined directly. After purging the TIC in the reactor with hydrochloric acid and the determination of the TIC content the sample boat is transferred into the combustion tube.

  • Page 44: Daily Factor

    Measuring methods multi EA 4000 For every parameter up to three calibration functions can be stored in a method. The allocation is automatic. The calibration function is calculated mass-related. Linear and quadratic calibration functions are calculated in accordance with the equations (5) and (6) through regres- sion calculation.

  • Page 45: Other Calculations

    multi EA 4000 Measuring methods The correlation coefficient compares the dispersion of the calibration measuring points Correlation coefficient of the regression function with the total dispersion of the calibration. If all calibration measuring points are on the calculated regression function, the correlation coefficient is +1 or -1.

  • Page 46: Data Analysis In The Cl Mode

    Measuring methods multi EA 4000 Data analysis in the Cl mode 4.7.1 End point routine After filling the measuring cell or after each change of the electrolyte solution an end point routine must be performed to define the operating point of the system. The indi- cation value determined represents both the starting point and the end point of titra- tion.

  • Page 47: Commissioning

    multi EA 4000 Commissioning Commissioning Site requirements 5.1.1 Installation conditions The following requirements are placed on the climatic conditions in the operating room of the analyzer:  Temperature range: +10 °C to +35 °C  Max. humidity: 90% at 30 °C ...

  • Page 48: Gas Supply

    Commissioning multi EA 4000 For the use of the basic device with the furnace module (HTS1500) in areas with mains voltages of 100 V/115 V/120 V/127 V a 2 phase connection is possible using optional accessories. Contact Analytik Jena AG if required. This installation may only be performed by the customer service department of Analytik Jena AG or by specialist per- sonnel authorized and trained by Analytik Jena AG! The installation of the electrical equipment of the laboratory must comply with the...

  • Page 49: Positioning The Analyzer With Various Detector Modules

    multi EA 4000 Commissioning Positioning the analyzer with various detector modules NOTICE Always switch off the multi EA 4000 before positioning! Connecting or disconnecting electrical contacts may damage the sensitive electronic components of the multi EA 4000 and detector modules. 5.3.1 Positioning the multi EA 4000 C/S For the combination multi EA 4000 - C/S module the following connections must be in...

  • Page 50: Figure 32 Multi Ea 4000 C/S

    Commissioning multi EA 4000 Hose diagram Figure 32 multi EA 4000 C/S...

  • Page 51: Positioning The Multi Ea 4000 Cl

    multi EA 4000 Commissioning 5.3.2 Positioning the multi EA 4000 Cl Connections multi EA 4000 connections Target "analyte out" Open outlet  "O " Oxygen gas connection  "Ar" Argon gas connection  Mains cable Mains connection  "com1" Cl module "COM" ...

  • Page 52: Figure 33 Multi Ea 4000 Cl

    Commissioning multi EA 4000 Hose diagram Figure 33 multi EA 4000 Cl...

  • Page 53: Positioning The Multi Ea 4000 C/S Cl

    multi EA 4000 Commissioning 5.3.3 Positioning the multi EA 4000 C/S Cl For the combination multi EA 4000 - C/S module - Cl module, the following connec- Connections tions must be in place: multi EA 4000 connections Target "analyte out" C/S module "analyte"...

  • Page 54: Figure 34 Multi Ea C/S Cl For C/S Measurements

    Commissioning multi EA 4000 Hose diagrams Figure 34 multi EA C/S Cl for C/S measurements...

  • Page 55: Figure 35 Multi Ea 4000 C/S Cl For Cl Measurements

    multi EA 4000 Commissioning Figure 35 multi EA 4000 C/S Cl for Cl measurements...

  • Page 56: Positioning The Automatic Tic Solids Module

    Commissioning multi EA 4000 5.3.4 Positioning the automatic TIC solids module For the combination multi EA 4000 - C/S module - Cl module, the following connec- Connections tions must be in place: multi EA 4000 connections Target "analyte out" TIC module "analyte (HT)" ...

  • Page 57: Figure 36 Automatic Tic Solids Module

    multi EA 4000 Commissioning Hose diagrams Figure 36 Automatic TIC solids module...

  • Page 58: Figure 37 Multi Ea 4000 C/S With Automatic Tic Solids Module

    Commissioning multi EA 4000 Figure 37 multi EA 4000 C/S with automatic TIC solids module...

  • Page 59: Positioning The Manual Tic Solids Module

    multi EA 4000 Commissioning 5.3.5 Positioning the manual TIC solids module For the combination multi EA 4000 - C/S module - TIC solids module, the following Connections connections must be in place: multi EA 4000 connections Target "analyte out" Open ...

  • Page 60: Figure 38 Multi Ea 4000 With Man. Tic Solids Module

    Commissioning multi EA 4000 Hose diagrams Figure 38 multi EA 4000 with man. TIC solids module...

  • Page 61: Figure 39 Multi Ea 4000 C/S Cl With Man. Tic Solids Module

    multi EA 4000 Commissioning Figure 39 multi EA 4000 C/S Cl with man. TIC solids module...

  • Page 62: Connecting And Using The Autosampler

    Commissioning multi EA 4000 Connecting and using the autosampler CAUTION There is a risk of burns at the hot the combustion furnace! Allow the basic device to cool down sufficiently before positioning and aligning the autosampler! During autosampler operation, there is a risk of burns at the hot boat and ceramic hook! After pulling out of the furnace, the boat and hook remain hot for a long time.
  • Page 63 multi EA 4000 Commissioning 6. Position the autosampler parallel to the basic device. The hook extension must be centered with the gas sluice. Move the autosampler to the basic device until the FPG 48 touches the spacers at the basic device. A gap of 2 mm then remains between the FPG 48 and the gas sluice to al- low for the compensation of thermal expansion of the combustion tube.
  • Page 64 Commissioning multi EA 4000 Position 1 1. 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 initial- ize the analyzer. 2. Select the menu command S ...
  • Page 65 multi EA 4000 Commissioning 8. Repeat the process until the gripper is positioned just a few millimeters below the boat storage. This prevents the boat from moving when picked up by the gripper. 9. Click on [ SAVE AND EXIT Sliding position The sliding position is the cut-out in the sliding rod of the ce- ramic hook.

  • Page 66: Installing The Boat Sensor

    Commissioning multi EA 4000 5.4.2 Installing the boat sensor The boat sensor monitors the boat transfer from the sampler FPG 48 to the furnace. It detects the following fault conditions:  Ceramic boat broken  No ceramic boat on the hook If one of the fault conditions occurs, the measurement is canceled immediately.

  • Page 67: Figure 40 Retrofit Kit For Fpg 48 To Use The Boat Storage

    multi EA 4000 Commissioning Boat storage Hexagon socket screws with washers Cover for sliding rod Figure 40 Retrofit kit for FPG 48 to use the boat storage 1. Unscrew the stop plate of the guide rail (1). 2. Remove the two hexagon socket screws (2). 3.

  • Page 68: Measurement Cancellation When Using The Sampler Fpg 48

    Commissioning multi EA 4000 A window with the same name opens. 12. In the area A place a tick for E CCESSORY MODULES JECTION RAIL 13. Adjust the position of the gripper relative to the ejection rail (→ see section "In- stalling and adjusting the autosampler FPG 48"...

  • Page 69: Connecting And Using The External Scales

    multi EA 4000 Commissioning Connecting and using the external scales When using the external scales the sample mass can be transferred directly to the se- quence table. 1. Connect the scales to the "scale" connection of the C/S module or Cl module. 2.

  • Page 70: Operation

    Operation multi EA 4000 Operation Activation / warm-up phase / setup CAUTION Crushing hazard at the autosampler FPG 48! The autosampler arm, the gripper and the boat carousel move during activation and initialization. Keep an adequate distance to avoid having your hands crushed. NOTICE In case of large temperature differences between storage and the installation wait un- til the multi EA 4000 has adapted to the ambient temperature before connecting it in...

  • Page 71: C/S Measurement

    multi EA 4000 Operation After successful login, automatic initialization and query of the components starts. The Warm-up and run-in current values are displayed in the status window: phases  Measuring gas flow: Appears after activation of the suction pump (100 ± 10 l/h). ...

  • Page 72: Figure 42 Ceramic Tube With Dust Trap And Gas Sluice

    Operation multi EA 4000 For C/S measurements a ceramic combustion tube is used. It is chamfered at both ends and symmetrical. The combustion tube is pushed into the gas sluice and the dust trap at the chamfered ends. Figure 42 Ceramic tube with dust trap and gas sluice Dust trap with cooling ribs Gas sluice with gas connection Chamfered ceramic tube...
  • Page 73 multi EA 4000 Operation 4. Insert the ceramic tube with gas sluice into the multi EA 4000 on the right-hand side. If the tube gets jammed, push it further without pressure by slightly rotating it. 5. Screw the gas sluice with 3 hexagon socket screws to the basic device.

  • Page 74: Performing The C/S Measurement

    Operation multi EA 4000 If the gas sluice has already been installed, the ceramic tube can also be inserted into the basic device from the left-hand side via the opening of the dust trap.  For ease of handling first place the dust trap onto the ceramic tube. ...
  • Page 75 multi EA 4000 Operation CAUTION Crushing hazard at the autosampler! The autosampler arm, the gripper and the boat carousel move during activation and initialization and measurement operation. Keep an adequate distance to avoid having your hands crushed. When filling the autosampler: Only open the cover when the boat carousel is no longer moving.
  • Page 76 Operation multi EA 4000 8. Click on [S TART MEASUREMENT 9. Create or select an analysis group for storing the measuring data. 10. Create an analysis sequence. Add the desired number of samples to the sample table with  Enter the following data: ...

  • Page 77: Determination Of Carbon After Pyrolysis

    multi EA 4000 Operation Determination of carbon after pyrolysis 6.3.1 Preparing the multi EA 4000 and C/S module CAUTION With pyrolysis volatile carbon compounds escape from the multi EA 4000. Attach an extraction pipe close to the furnace inlet and ensure that the pyrolysis gas is extracted. 1.
  • Page 78 Operation multi EA 4000  The status lights at the front of the devices illuminate. Do not switch any Cl module present. If present, switch on the automatic TIC solids module from the mains switch at the rear. 2. Start the multiWin program. 3.
  • Page 79 multi EA 4000 Operation With an automatic sample ID can be created. Selection of the analysis type (S NALYSIS TYPE AMPLE AILY FACTOR DETERMINATION , AQA or D ALIBRATION MEASUREMENT MEASUREMENT BOAT BLANK Target concentration for calibration standards or AQS standard OMINAL VALUE Input of the sample weight PERANDS...

  • Page 80: Cl Determination

    Operation multi EA 4000 Cl determination 6.4.1 Preparing the multi EA 4000 for Cl measurements WARNING Risk of electric short circuit! In the combustion furnace HTS1500 very high electrical currents occur in spite of a low voltage (max. 14 V). The combustion tube is part of the cover of live components.

  • Page 81: Figure 45 Coupling Element For Cl Measurements

    multi EA 4000 Operation Figure 45 Coupling element for Cl measurements Check the electrical connections and hose connections according to section "Position- ing the multi EA 4000 Cl" or "Positioning the multi EA 4000 C/S Cl" p. 51ff. 1. Fill the quartz tube with approx. 2.5 cm quartz wool and push the cotton plug into the end of the tube.
  • Page 82 Operation multi EA 4000  The gas sluice is correctly assembled if the gap be- tween the pressure ring and the matching piece is evenly approx. 1 mm wide. 5. Fit the coupling element with three hexagon socket screws to the right side of the basic device. Make sure that the guide hole is above the slot in the basic device and the re- cess points towards the front.
  • Page 83 multi EA 4000 Operation Connecting the flame sensor (optional) 1. Assemble the flame sensor: Consecutively insert the 2 sealing rings (3) and the brass sleeve (4) into the sensor head (1). Screw the aluminum knurled head screw (5) only lightly to the sensor head. Note: A third seal is included with the flame sen- sor as a replacement.
  • Page 84 Operation multi EA 4000 1. Screw the PTFE tray and the 2 clamps for the safety container to the basic device, if applicable. 2. Fill the sulfuric acid container with 12-15 ml sulfu- ric acid. 3. Hold the filled sulfuric acid container above the PTFE tray.
  • Page 85 multi EA 4000 Operation Only sulfuric acid containers with split outlet: 8. Connect the split outlet of the sulfuric acid con- tainer (1) via a short piece of hose to the lateral connection of the safety container (2). 9. Press the safety container into the 2 clamps. 10.

  • Page 86: Preparing The Electrolyte Solution

    Operation multi EA 4000 6.4.2 Preparing the electrolyte solution WARNING The 99% acetic acid and nitric acid and thymol used to prepare the electrolyte solution can cause severe chemical burns! Wear the appropriate protective clothing when preparing the electrolyte solution! Ob- serve all specifications in the safety data sheets! Reagents required: ...

  • Page 87: Preparing The Measuring Cell

    multi EA 4000 Operation 6.4.3 Preparing the measuring cell NOTICE If the electrolyte dries on the combined electrode, it can damage the electrode. During brief interruptions in operation, e.g. overnight, store the electrode in electrolyte solu- tion. Leave the electrode for 1-2 h in electrolyte solution prior to first use. Reproducible val- ues are only possible after that.

  • Page 88: End Point Routine

    Operation multi EA 4000 6.4.4 End point routine An end point routine is necessary after every electrolyte change. The operating point of the coulometric measuring cell is in the range of 1500-5000 counts. 1. Start the end point routine via the menu item S ...
  • Page 89 multi EA 4000 Operation 3. Change between the various analyzer modules. To do so, first activate the sensors: Select the menu command D  D – E EVICE EVICE  Enable chlorine as E to be analyzed. LEMENT  If both carbon/sulfur and chlorine are enabled, click on Q (C) in the UARTZ TUBE ...
  • Page 90 Operation multi EA 4000 Gas flows for measurements with measuring gas split pump max. (approx. 2.5 l/min) 1 l/min 2.4 l/min First transfer the split factor from an existing method and then recalculate it. 3. Weigh the samples onto the quartz boats. Samples, such as used oil, should be placed on annealed quartz sand during weigh- ing into the quartz glass boat and covered with a sufficient quantity of quartz sand.

  • Page 91: Checking The Split Ratio

    multi EA 4000 Operation Use manual sample feed CAUTION When feeding the furnace whilst simultaneously monitoring combustion protective goggles must be used.  Start the measurement. Then move the boat into the furnace.  Move the boat into the combustion tube up to just behind the gas sluice so that the center of the boat is at the height of the front plate.

  • Page 92: Burning Off Quartz Boats

    Operation multi EA 4000 Enter the calculated factor in the method on the tab C in the input  ALIBRATION field D . Accept the value with [A ] for the subsequent measure- AY FACTOR CCEPT ments. For the calculation of a new split factor the day factor must be set to a value of 1 n the method on the tab C ALIBRATION 6.4.7...

  • Page 93: Figure 46 Components For Connecting The Tic Reactor And Ceramic Tube

    multi EA 4000 Operation Figure 46 Components for connecting the TIC reactor and ceramic tube Base element of the gas sluice Sealing rings (in the Figure with black sealing ring for the pressure Knurled ring ring) Pressure ring The gas connection at the base element (1 in Figure 46) remains unattached during measurements with the automatic TIC solids module.
  • Page 94 Operation multi EA 4000 If the tube gets jammed, push it further without pres- sure by slightly rotating it. Insert the tube firmly into the seal of the gas sluice. 5. Place the dust trap contact guard on the left-hand side of the basic device.
  • Page 95 multi EA 4000 Operation 5. Secure the ceramic cannula with the red screw cap. 6. Check that the sealing cone, seals and screw cap have been fitted to the pump hose. 7. Screw the pump hose finger-tight onto the red screw cap. NOTICE! The TIC reactor can get hot.

  • Page 96: Reagents Required

    Operation multi EA 4000 12. Slice the white PTFE ring onto the end of the TIC reactor. 13. Position the sampler FPG 48 and retrofit the boat storage (→ see section "Installing and adjusting the autosampler FPG 48" p. 62). Move the sampler towards the TIC solids module.
  • Page 97 multi EA 4000 Operation Select the menu command D  D –  EVICE EVICE EDIT Enable "C" in the list E LEMENTS  In the list C click on C (CS). OMBUSTION TUBE ERAMIC TUBE  As S enable the option TATES SOLID ...

  • Page 98: Toc Determination Based On Differentiation Method

    Operation multi EA 4000 Populate the autosampler. Use the buttons to move the sample  rack to the desired position. Click on in the sequence row to release it for analysis. All sequence rows can  be released by clicking on the button.
  • Page 99 multi EA 4000 Operation Select the menu command D  D –  EVICE EVICE EDIT Enable "C" in the list E LEMENTS  In the list C click on C (CS). OMBUSTION TUBE ERAMIC TUBE  As S enable the option TATES SOLID ...
  • Page 100 Operation multi EA 4000 Click on in the sequence row to release it for analysis. All sequence rows can  be released by clicking on the button.  Sequence rows released for analysis have a green fill. 12. Click on [S TART MEASUREMENT ...

  • Page 101: Toc Measurement Using Direct Determination

    multi EA 4000 Operation 6.5.5 TOC measurement using direct determination CAUTION During autosampler operation there is a risk of burns at the hot boat and ceramic hook! After pulling out of the furnace the boat and hook remain hot for a long time. CAUTION Crushing hazard at the autosampler! The autosampler arm, the gripper and the boat carousel move during activation and initialization and measurement operation.
  • Page 102 Operation multi EA 4000 pump Ar/O approx.1.7 l/min 2.5 l/min 1.5 l/min corresponds to N OMINAL 100 ± 10 in the S TATUS ANA- window LYZER The analysis system now has time to settle down. If the intake flow differs greatly or changes later, readjust the intake flow at the "pump"...

  • Page 103: Tic Determination With The Manual Tic Solids Module

    multi EA 4000 Operation The measuring gas from the purged TIC is passed via the measuring gas drying  and cleaning of the automatic TIC solids module to the detector in the C/S module. The same boat is then moved further into the furnace to determine the TOC ...
  • Page 104 Operation multi EA 4000 In addition to the safety instructions for the analyzer multi EA 4000 provided in sec- tion "Safety instructions" p. 10, the following instructions also apply specifically when operating the manual solids module: CAUTION The reactor vessel and the hoses for supplying acid contain phosphoric acid! Phos- phoric acid is irritating to eyes, skin and mucous membranes! Perform slow metering operations with the dispenser to avoid overpressure! Wear protective gloves and protective goggles when handling concentrated acid! Rinse...
  • Page 105 multi EA 4000 Operation In the method on the P tab set the furnace temperature to a value of 0 °C. ROCESS This means the combustion furnace is not monitored and the analyzer released for the measurement. 9. Adjust the oxygen flow at the valve to 16 l/h. 10.
  • Page 106 Operation multi EA 4000 Slowly adjust the stirrer to stage 5. The sample must not be spun against the  wall of the flask. Jolting or rapid movement of the stirrer must therefore always be avoided. Add 2 ml acid evenly 1-3 times (dependent on the concentration and sample ...

  • Page 107: Maintenance And Care

    multi EA 4000 Maintenance and care Maintenance and care Maintenance and care of the analyzer are described in this section separately for the individual modules. Observe the notes for all modules combined in your system. Basic device multi EA 4000 Maintenance intervals Maintenance task Maintenance interval...

  • Page 108: Operation With C/S Module

    Maintenance and care multi EA 4000 Operation with C/S module Maintenance intervals Maintenance task Maintenance interval Inspect ceramic tube for cracks and visible Every three months damage, replace if necessary Inspect and clean dust trap Monthly (dependent on combustion and sample matrix) Inspect the dust filter, replace in case of visible Monthly (dependent on combustion and...
  • Page 109 multi EA 4000 Maintenance and care 4. Detach the measuring gas hose (hose no. 1) from the dust trap. 5. Slightly pull the dust trap to detach it. NOTICE! The dust trap might come loose abruptly. Sup- port yourself with your hands when pulling. The ceramic tube might come loose with the dust trap.

  • Page 110: Cleaning The Dust Trap

    Maintenance and care multi EA 4000 2. Detach the 3 fastening screws for the gas sluice and remove the gas sluice. 3. Remove the fractured parts of the ceramic tube from the furnace. NOTICE! The heating elements of the furnace must not be damaged when remov- ing fractured pieces! 1.

  • Page 111: Figure 48 Dust Filter

    multi EA 4000 Maintenance and care  when the pump flow drops as an indication of clogging Check monthly whether the dust filter on the front of the device is clogged. If so, re- place the dust filter and clean the dust trap. Figure 48 Dust filter 1.

  • Page 112: Changing The Desiccant In The Drying Tube

    Maintenance and care multi EA 4000 10. Place the dust trap onto the ceramic tube and align it with the gas connection pointing up. Press the dust trap slightly against the tube towards the tube axis until the dust trap slips onto the tube and cannot be moved fur- ther.

  • Page 113: Replace The Halide Trap

    multi EA 4000 Maintenance and care 7.2.4 Replace the halide trap Halide traps are used in the following measurement arrangements:  TC measurement at the multi EA 4000 basic device  Cl measurement in the Cl module  TIC measurement: in the corresponding TIC solids modules NOTICE Risk of damage to optical and electronic components (detectors, flow sensors) from aggressive combustion products if the copper wool in the halide trap is used up!

  • Page 114: Operation With Cl Module

    Maintenance and care multi EA 4000 Operation with Cl module Maintenance intervals Maintenance task Maintenance interval Remove splashes of chemicals from the Immediately housing Inspect the combustion tube and replace After approx. 100 operating hours if necessary Clean measuring cell At least weekly Recommendation: wipe clean after electrolyte replacement...

  • Page 115: Servicing/Replacing The Quartz Glass Combustion Tube

    multi EA 4000 Maintenance and care 6. Rinse the sulfuric acid container with a small amount of fresh sulfuric acid. If heav- ily contaminated, rinse the sulfuric acid container several times with ultrapure wa- ter and allow it to dry fully. 7.
  • Page 116 Maintenance and care multi EA 4000 1. Switch off the basic device from the mains switch, pull the mains switch out of the outlet and discon- nect the gas supply. 2. Pull the gas olive out of the sulfuric acid container. When using the safety container: Pull the black hose off the bypass of the sulfuric acid container.

  • Page 117: Servicing The Combined Electrode

    multi EA 4000 Maintenance and care 13. Place approx. 2.5 cm quartz wool in the inlet of the quartz tube and push the quartz wool towards the end of the tube with a hook. 14. Refit the gas sluice and insert the combustion tube into the furnace. Restore all gas connections (→...

  • Page 118: Servicing The Measuring Cells

    Maintenance and care multi EA 4000 Correct Incorrect Hold the electrode from the top and pull the Do not pull and jolt the lateral connection electrode straight upwards out of the cover. sleeve for the electrical connections. The con- nections in the sleeve will break (not visible from outside)! Correct Incorrect...

  • Page 119: Replacing The Adsorption Agent

    multi EA 4000 Maintenance and care Observe the following notes:  If the system is decommissioned for several days, clean the measuring cell and store it dry.  Regularly check the casing of the magnetic stirring rod for cracks. Metal ions enter- ing the electrolyte solution can distort the analysis.

  • Page 120: Cleaning The Tic Reactor Of The Automatic Tic Solids Module

    Maintenance and care multi EA 4000 Maintenance task Maintenance interval Clean the condensation coil As required, but no later than after 12 Months Inspect the condensate container for damage After 3 months Clean the condensate container As required, but no later than after 12 months Replace the metering pump, pump hose After 3 months...

  • Page 121: Cleaning The Condensation Coil

    multi EA 4000 Maintenance and care 4. Put the acid container and drip tray aside. Care- fully wipe the pump hose clean. NOTICE! The acid from the hose must not drip onto the device. 5. Unscrew the connection for the acid supply (1) from the TIC reactor.

  • Page 122: Removing And Replacing The Pump Hose

    Maintenance and care multi EA 4000 4. Pull the hoses off the condensation coil. 5. Carefully pull the condensation coil out of its mount. 6. Inspect the condensation coil for deposits and cracks. 7. If necessary, rinse the condensation coil with ul- trapure water and allow to dry well.

  • Page 123: Figure 49 Clamping The Pump Hoses

    multi EA 4000 Maintenance and care 4. Pull the sealing elements and the white union nut off the worn pump hose. 5. Slide the sealing elements onto the new pump hose in the se- quence shown. Figure 49 Clamping the pump hoses Phosphoric acid bottle Hose cartridge Stopper at the pump hose...
  • Page 124 Maintenance and care multi EA 4000 1. Push the bracket on the condensate pump to the left. 2. Pull the hoses no. 77 and no. 78 off the connections. 3. Remove the conveyor belt with the pump hose from the pump body. 4.

  • Page 125: Cleaning The Condensate Container

    multi EA 4000 Maintenance and care 7.4.4 Cleaning the condensate container Clean the condensate container as required: 1. Detach the 2 knurled head screws (arrow) at the cover of the cooling block and remove the cover. 2. Pull the hoses off the connections of the condensate container. 3.

  • Page 126: Cleaning The Tic Reactor At The Manual Tic Solids Module

    Maintenance and care multi EA 4000 7.5.1 Cleaning the TIC reactor at the manual TIC solids module After each measurement, rinse the TIC reactor (Erlenmeyer flask) with ultrapure wa- ter. Next dry it thoroughly (see also "Performing a TIC measurement" p. 103). Replacing the water traps NOTICE The water traps (TC prefilter and disposable retention filter) can be replaced in the...

  • Page 127: Fault Removal

    multi EA 4000 Fault removal Fault removal General information For fault analysis it is possible to record log files. The recording of log files should be enabled in coordination with the Analytik Jena AG customer service department.  Enable the recording of the device-specific log files multiWin_Comm.log and multi- Win_Flow.log under E ...
  • Page 128 Fault removal multi EA 4000 Serial port not present! Cause Remedy Communication problems  Disconnect USB connection between the control module and PC and re-connect after approx. 10 s  Initialize Serial port not reachable! Cause Remedy Communication problems  Disconnect USB connection between the control module and PC and re-connect after approx.
  • Page 129 multi EA 4000 Fault removal Data transfer interrupted Cause Remedy no data transfer for 10 s  Initialize Incorrect interface protocol ID Cause Remedy Fault after update  update required (program versions of firmware multiWin don't match) Timeout: InitEnd Cause Remedy timeout during initialization ...
  • Page 130 Fault removal multi EA 4000 Command from the PC not complete Command from the PC without STX Command from the PC CRC error Command from the PC invalid command Command from the PC invalid MEAS command Command MTXT from PC missing Cause Remedy communication error...
  • Page 131 multi EA 4000 Fault removal S sensor: inactive Cause Remedy Detector type transfer failed  Repeat action Cl sensor: no connection Cause Remedy  Acknowledge message Communication faulty after detector was detected during initialization  Initialize Cl sensor: incorrect command structure Cause Remedy communication to the chlorine module faulty...
  • Page 132 Fault removal multi EA 4000 pressure missing Cause Remedy flow inadequate  Check O connection  Check pressure Ar pressure missing Cause Remedy Argon flow inadequate  Check argon connection  Check pressure Sampler: no connection Cause Remedy Communication faulty after sampler was detected dur- ...

  • Page 133: Displays In The D

    multi EA 4000 Fault removal Displays in the D window EVICE TATUS In the D window, information on the device status or individual modules is EVICE TATUS displayed. Figure 50 Window S TATUS ANALYZER Method Flow indication (not for Cl measurements) Analysis module / sampler Temperature indication Detection/sensor module...
  • Page 134 Fault removal multi EA 4000 The respective status of the detector modules is indicated by color (see above). The following status displays are possible: Device ready for measurement Display Description OK (green, black) Detector is ready for measurement Device not ready for measurement - general Display Description no detector displayed...

  • Page 135: Equipment Fault

    multi EA 4000 Fault removal Equipment fault Other problems not detected by the system monitoring can also occur. Starting a measurement is possible. Such errors are usually detected on the basis of implausible measuring results (analytical problems). Often, they are clearly recognizable in the equipment technology.

  • Page 136: Cl Module

    Fault removal multi EA 4000  Pump not switched on.  Wait for the temperature difference between target and actual temperature to approximate 50 K. If the pump does not activate at a temperature differ- ence between target and actual temperature of less than 50 K, inform Service.

  • Page 137: Device Communication Fault

    multi EA 4000 Fault removal multiWin: no connection to Cl sensor Cause Solution  No communication between the internal computer and Observe activation sequence: coulometer. 1. Switch on basic device.  Cl module not switched on. 2. Switch on Cl module. 3.

  • Page 138: Analytical Problems

    Fault removal multi EA 4000 multiWin: Communication error - incorrect command set between PC and device Cause Solution  Internal and external program versions do not match.  Repeat update. multiWin: no connection to temperature controller Cause Solution  Basic device not switched on. ...

  • Page 139: Cl Determination

    multi EA 4000 Fault removal High results for TC Cause Solution  Combustion tube is cracked or broken.  Ambient air can enter the system through cracks leading to significant high results for TC. In this case, replace combustion tube. Baseline drift Cause Solution...

  • Page 140: Tic Determination (Automatic Tic Solids Module)

    Fault removal multi EA 4000 8.6.3 TIC determination (automatic TIC solids module) Lower results Cause Solution  Sample weight chosen too high  The sample weight should not exceed 50 mg, otherwise the metered acid volume (400 µl) is not enough to fully digest the carbonate or the acid volume cannot fully wet the sample.

  • Page 141: Measurements In Pyrolysis Mode (Ec)

    multi EA 4000 Fault removal 8.6.5 Measurements in pyrolysis mode (EC) Low results of elementary carbon (after pyrolysis) Cause Solution  Waiting period for purging oxygen by argon in the com-  The waiting period after changing from oxygen to argon bustion tube chosen too short supply should be min 60 s.

  • Page 142: Transport And Storage

    Transport and storage multi EA 4000 Transport and storage Transport 9.1.1 Preparing the analyzer for transport WARNING Risk of damage to health due to improper decontamination! Perform a professional and documented decontamination of the device before return- ing it to Analytik Jena. The decontamination report is available from Service when reg- istering the return.
  • Page 143 multi EA 4000 Transport and storage 8. Remove the heating elements and the furnace cartridge from the multi EA 4000 and package these device components separately (→ see section "Removing the heating elements and furnace cartridge" p. 144). 1. Switch off the C/S module from the mains switch. C/S module 2.

  • Page 144: Removing The Heating Elements And Furnace Cartridge

    Transport and storage multi EA 4000 9.1.2 Removing the heating elements and furnace cartridge WARNING Life-threatening electrical voltages and high currents may occur in the interior of the analyzer! For the removal of the heating elements and furnace cartridge witch off the analyzer from the mains switch at the rear of the device and disconnect the mains plug from the mains outlet.
  • Page 145 multi EA 4000 Transport and storage 5. Detach the protective conductor (5) from the furnace cartridge (4) and the L-shaped mounting plate (3). 6. Detach the orange connection cable of the thermocouple (1) and the green ground conductor (2) from the inside wall of the basic device.

  • Page 146: Transport Notes

    Transport and storage multi EA 4000 13. Successively lift out the heating elements carefully from the furnace cartridge. 14. Package the two heating elements and the braided wire and the furnace cartridge in separate transport contain- ers. 9.1.3 Transport notes Observe the safety instructions in section "Safety instructions, transport and "...

  • Page 147: Storage

    multi EA 4000 Transport and storage  For reasons of safety 2 persons are required to transport the analyzer and must position themselves on both sides of the equipment.  Because the analyzer does not feature any handles, firmly grip the device from the bot- tom and make sure prior to simultaneous lifting the device that the sensitive components at the front are protected by the closed doors.

  • Page 148: Disposal

    Disposal multi EA 4000 Disposal The used desiccant of Cl determination is initially carefully diluted with water and then Sulfuric acid neutralized with sodium hydroxide. The corresponding hazard information and safety advice must be observed! This neutralized waste must be brought to the appropriate waste disposal center for correct disposal according to the appropriate legal guidelines.

  • Page 149: Specification

    multi EA 4000 Specification Specification 11.1 Technical data General characteristics Designation/type Analyzer multi EA 4000 Dimensions Basic device (W x H x D) 600 x 470 x 620 mm each module: 300 x 470 x 550 mm Autosampler: 520 x 500 x 700 mm Mass approx.
  • Page 150 Specification multi EA 4000 Maximum power consumption HTS1500 furnace module 2400 VA C/S module 60 VA Cl module 60 VA Autosampler FPG 48 30 VA Autom. TIC solids module 20 VA Man. TIC solids module 415 VA Overall system approx. 3000 VA PC interface Environmental conditions Temperature during storage...

  • Page 151: 11.2 Standards And Directives

    multi EA 4000 Specification 11.2 Standards and directives The analyzer has a protection class of I. Protection class and type of protection The housing has safety type IP 20. The analyzer complies with the safety standards Device safety  EN 61010-1 ...

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