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EOX determination

multi X 2500

7.1.3

Performing measurements

WARNING

Concentrated sulfuric acid and concentrated acetic acid can cause severe chemical

burns! Wear the appropriate protective clothing when pouring the electrolyte solution!

Observe all instructions and specifications in the safety data sheets!

Fill fresh sulfuric acid into the sulfuric acid container with outlet on the chlorine

module every day (

→

"Changing the sulfuric acid and cleaning the sulfuric acid

container with outlet", p. 101).

Preparing the measuring cell:



Top up the measuring cell with fresh electrolyte solution every day.
Measuring cell "high sensitive": approx. 65 ml



Insert the magnetic stirring rod into the measuring cell. Fit the cover.



Insert the electrodes and connect them electrically.



Connect the measuring gas hose from the sulfuric acid container to the gas

inlet tube using the Teflon screw connection.



Connect the adapter to the extraction hose.

NOTICE! Do not connect the measuring cell "high sensitive" to the intake pump.

Otherwise, electrolyte could get drawn into the pump.

The analyzer and the chlorine module are switched on.



The devices are booted. The status LEDs on the front panel lights up in green

after approximately 30 seconds.

Open the gas supply and set the primary pressure to 4 to 6 bar.

Switch on the PC.

Start the control and analysis software multiWin and log in with user name and
password.

Initialize the analysis system by clicking on [

INITIALIZE ANALYZER



The initialization and automatic detection of all connected components will be
executed.

In the window D

EVICE STATUS

any components not yet ready for operation will be

shown in red. The time it takes to preheat the furnace to 950 °C is about 30 to

40 min. During the warm-up phase it is not possible to start a measurement.
If the analyzer is still not ready for measurements after about 40 min., carry out a
fault analysis in accordance with the notes in chapter "Fault removal" on page 106.

Carry out an end point routine to adjust the electrolyte to the optimal operating

range of the measuring cell.

If necessary, test the measuring cell using a direct method.

10.

Providing the samples:

Load the EOX/liquids rack of the autosampler autoX 112 with samples.

Содержание Analytik Jena Multi X 2500

Страница 1: ...Operating Manual multi X 2500 ...

Страница 2: ...de http www analytik jena com multi X and multiWin are registered trademarks of Analytik Jena AG in Germany Microsoft and Windows are registered trademarks of Microsoft Corp The identification with or TM is omitted in this manual 11 889 691 01 17 Analytik Jena AG Copyright 2017 Analytik Jena AG Manufacturer Service General information Copyrights and Trademarks Documentation number Edition Implemen...

Страница 3: ...ation 17 3 3 System design 17 3 4 Layout of the multi X 2500 18 3 4 1 Electronic components 18 3 4 2 Gas supply measuring gas transfer 21 3 4 3 Combustion system 24 3 4 4 Measuring gas drying in the standard version 26 3 4 5 Auto protection assembly optional 26 3 5 Chlorine module multi X 2500 28 3 5 1 Connections and interfaces 30 3 5 2 Measuring cell sensitive default 31 3 5 3 Measuring cell hig...

Страница 4: ...1 Removing and cleaning the open combustion tube 89 10 3 2 Change the sulfuric acid and clean the sulfuric acid container vertical 91 10 3 3 Replace the activated carbon in the adsorption tube 92 10 3 4 Servicing the measuring cell 92 10 3 5 Clean and store the combined electrode 93 10 4 Maintenance activities optional version 93 10 4 1 Checking the settings of the gas flows 93 10 4 2 Checking the...

Страница 5: ...chlorine module 30 Fig 20 Terminal on the internal wall of the chlorine module 31 Fig 21 Measuring cell sensitive with lid 31 Fig 22 Loaded measuring cell sensitive 32 Fig 23 Electrode for sensitive high concentration measuring cells 32 Fig 24 Measuring cell high concentration 33 Fig 25 Measuring cell high sensitive 34 Fig 26 Loaded measuring cell high sensitive 34 Fig 27 Sensor electrode 35 Fig 2...

Страница 6: ...ulti X 2500 6 Fig 45 Connections on the POX sluice 85 Fig 46 Connection of the argon hose to the basic device and the POX container 86 Fig 47 Flow monitoring set 94 Fig 48 Connection of the flow monitoring set 95 ...

Страница 7: ... g FILE OPEN These instructions are aimed at qualified specialist users with knowledge of the analysis of sum parameters The instructions are limited to describing the functionality of multi X 2500 and its accessories For the safe operation of the multi X 2500 knowledge of the operating instructions of the control and analysis software multiWin is also required Basic knowledge of working with a co...

Страница 8: ...nual Any other use is not as intended Only the operator is liable for any damages that result from this 1 3 Warranty and liability The warranty duration and liability comply with the legal requirements and the provisions in the general terms and conditions of Analytik Jena Deviations from the intended use described in this user manual result in limitations of warranty and liability in the event of...

Страница 9: ...n have to be observed and complied with References to potential dangers do not replace the work protection regulations which must be observed 2 1 1 Safety labeling on the multi X 2500 Warnings and information symbols have been attached to the multi X 2500 These must be observed under all circumstances Damaged or missing warnings and information symbols can cause incorrect actions leading to person...

Страница 10: ...pose a risk of injury During transport the components of the equipment must be secured in accordance with the instructions in the user manual The combustion furnace auto protection assembly all components made of glass and the measuring cell must be removed before transporting the device Only transport the analyzer in its original packaging Ensure that the transport protections have been fitted an...

Страница 11: ...must be in good working condition Covered ventilation grilles or slits etc may cause the device to break down or may cause damage to it The furnace operates with temperatures of up to 1100 C The hot components must not be touched during or directly after the operation of the analyzer Caution when handing quartz glass and glass parts Risk of broken glass and therefore risk of injury Prevent any ing...

Страница 12: ...ing the device switch on the rear of the housing and the power supply disconnected from the mains if there is any interference with the electric components 2 4 3 Safety instructions for compressed gas containers and systems The carrier gas argon and oxygen is taken from compressed gas cylinders or local compressed gas systems Make sure that the carrier gas has the specified purity refer to Technic...

Страница 13: ... with quartz wool avoid the creation of dust Inhaled dust might cause irritation to respiratory tracts 2 4 5 Safety instructions service and repair The analyzer is usually serviced by the customer service department of Analytik Jena or its authorized and trained specialist personnel Independent servicing can lead to maladjustment or damage to the analyzer Therefore the operator may generally only ...

Страница 14: ...working with the optional version There is a risk of injury from sulfuric acid In case of an emergency shutdown the vacuum which builds up during the cooling down period may draw sulfuric acid into the gas transfer pipes and the auto protection assembly If possible disconnect the gas transfer line from the sulfuric acid container in the chlorine module before cutting the gas supply After an emerge...

Страница 15: ...ses at the same time The pyrolysis gases are dried with concentrated sulfuric acid 3 Detection of the hydrogen halides HCl HBr HI via micro coulometric titration HF is not determined This process will take place in an acetic acid medium in accordance with the following reaction equation 2 Ag X AgX 2 The silver ions needed for halide precipitation are produced electrolytically on a silver anode Whe...

Страница 16: ... the oxygen stream In the chlorine module the hydrogen halides which are produced are absorbed in the electrolyte solution The halide ions are determined argentometrically Two possible methods for absorbing the activated carbon are Column method Batch method Another possible method is the stirring method or carbodisc method which is not described in further detail in this manual The prepared water...

Страница 17: ...uced will then be absorbed before the halide ions are determined argentometrically 3 3 System design The standard version of the analyzer is composed of the following components multi X 2500 with combustion system chlorine module detector PC with multiWin software for device control and data analysis The standard version of the multi X 2500 uses the vertical operating mode and the sensitive measur...

Страница 18: ...o unhinge and reinsert the front doors to allow for better access to the device interior The mains connection the gas terminals and the interface for the system components are located on the rear of the device Fig 1 Front view with open doors 1 Furnace 2 Knob for tilting the furnace 3 Fan 4 Control electronics cover 5 Slots 6 Tilt device furnace 7 Collection tray with sulfuric acid container verti...

Страница 19: ... the device The computer is connected via a USB port The interfaces for connecting the autosampler and the detector module are RS 232 ports Fig 3 Rear view multi X 2500 1 Interfaces see Fig 4 2 PC connection via USB 3 Mains connection equipment switch The equipment fuse and the mains connection are located below the device s mains switch The rating plate is also attached there Mains connection and...

Страница 20: ...for power supply controlling the individual components of the basic device and the communication with the computer and other connected system modules The electrical connections of the combustion furnace the flame sensor and the thermocouple are located right under the control electronics cover The connections are only accessible in the vertical installation position of the combustion furnace Fig 5...

Страница 21: ...opening and closing the pneumatic seal in the auto protection assembly 2 Heating connection for gas transfer line 3 Connection auto protection assembly 3 4 2 Gas supply measuring gas transfer The gas connections are located on the rear of the device The gas supplies for oxygen and argon must be connected via the connection hoses included in the scope of delivery 6 x 4 mm to the connections IN O2 o...

Страница 22: ...ABD gas outlet 6 in Fig 7 is also used for the NPOC purge gas flow In the multi X 2500 the two process gases oxygen and argon are controlled via the gas box The gas box is located on the left side inside the device Fig 8 Gas box The O2 supply on the open combustion tube is effected via the oxygen sluice inserted into the opening of the combustion tube The gas outlet of the combustion tube is direc...

Страница 23: ...on tube 4 Oxygen sluice 5 O2 connection hose 3 open combustion tube The multi purpose combustion tube requires oxygen as the combustion gas and argon as the carrier gas The composition of the gas mixture for optimum gas digestion is controlled via the flow management system FMS Fig 10 Connections on the multi purpose combustion tube in horizontal mode 1 Ar connection hose 4 2 O2 connection hose 3 ...

Страница 24: ...ing analyses AOX determination in vertical operating mode recommended POX determination A quartz glass wool plug is located in the bottom of the combustion tube The quartz glass wool filters ashes and soot from the measuring gas stream When inserting the quartz container the plug cushions and prevents damaging the quartz glass Fig 12 Open combustion tube 1 Combustion tube 2 Gas outlet with spheric...

Страница 25: ...on for flame sensor 3 Screw cap with septum for EOX determination only 4 Oxygen supply connection The connection between the combustion tube and the additional measuring gas drying or downstream measuring gas path is implemented via the auto protection assembly The flame sensor is a recommended option for operating the automatic boat feeder ABD in horizontal mode The flame sensor controls the spee...

Страница 26: ...e pump in the chlorine module transfers the measuring gas to the measuring cell Fig 15 Sulfuric acid container vertical in the standard version 1 Gas outlet combustion tube 2 Sulfuric acid container vertical with plug 3 Measuring gas outlet to the chlorine module There is a particular sulfuric acid container that is mounted to the chlorine module which can be used with the optional multi purpose c...

Страница 27: ...c seal 6 Cable for electrical connection The coupling connects the combustion tube and the measuring gas transfer line The combustion tube is inserted into the auto protection assembly and sealed with a pneumatic seal The pneumatic seal is operated with argon The pneumatic seal is opened or closed with a toggle switch Toggle switch down Combustion tube sealed Toggle switch up Combustion tube relea...

Страница 28: ... and potentiometric titration Stirrer cooling block for the measuring cell with automatic cell detection Measuring cell with electrodes with gas inlet tube Intake pump Adsorption tube Sulfuric acid container for the operation with multi purpose combustion tube In the standard version the intake pump draws the measuring gas from the multi X 2500 directly into the measuring cell of the chlorine modu...

Страница 29: ...dule has 3 operative ranges A particular measuring cell is used for each operative range sensitive default high concentration optional high sensitive optional For further information on the measuring ranges of the measuring cells refer to Technical data on page 122 The measuring cells are automatically detected when they are inserted into the stirrer cooling block When the chlorine module is switc...

Страница 30: ...ion a different outlet must be connected to the extraction Outlet exhaust 2 in Fig 19 Outlet of the intake pump with filter standard version Outlet waste 3 in Fig 19 Outlet of the exhaust air hose optional version The filter on the exhaust outlet creates a vortex in the exhaust gas stream which reduces the noise level Fig 19 Connections on the rear of the chlorine module 1 Interface to the basic d...

Страница 31: ... and 100 µg The measuring cell consists of the electrode space which takes the electrolyte solution and the stirrer block in the chlorine module A generator anode in the form of a stable silver plate silver circle is located on the floor of the electrode space The magnetic stirring rod runs above the anode The cell is sealed airtight with a cover and three knurled head screws The two cover penetra...

Страница 32: ...ion It combines the indicator electrodes Ag the generator cathode Pt and the gas inlet The measuring gas hose can be connected directly to the electrode The combination electrode is dried and stored in the storage container in the front door after the measurement Fig 23 Electrode for sensitive high concentration measuring cells 1 Connector 2 Measuring gas hose connection 3 Gas inlet to the measuri...

Страница 33: ...ilar to the measuring cell sensitive this cell also uses a maintenance free combined electrode 3 5 4 Measuring cell high sensitive The optional measuring cell high sensitive is used for very low chlorine contents between 0 01 and 10 µg Cl in combination with the multi purpose combustion tube It is particularly recommended for EOX determinations The measuring cell high sensitive cannot be used in c...

Страница 34: ... to the extraction connection Fig 26 Loaded measuring cell high sensitive 1 Gas inlet tube with screw connection for measuring gas 2 Adapter to the extraction connection 3 Sensor electrode with pre amplifier 4 Opening for the direct injection with plug 5 Silver electrode 6 Platinum electrode with salt bridge 7 Measuring cell The sensor electrode combines the indicator and the reference electrodes ...

Страница 35: ...ensor electrode 1 Reference electrode 2 Refilling port for internal electrolyte Na2SO4 with rubber plug 3 Diaphragm 4 Silver ring sensor A pair of generator electrodes consisting of a platinum cathode with salt bridge and a silver anode is used to produce the silver ions required for chemical precipitation Fig 28 Pt electrode with salt bridge generator cathode 1 Pt electrode with salt bridge compl...

Страница 36: ...o the front door of the chlorine module It must be filled with 2 to 3 ml of internal electrolyte Fig 30 Chlorine module with measuring cell high sensitive 1 Gas transfer line from basic device 2 Sulfuric acid container with outlet and safety attachment 3 Measuring cell high sensitive 4 Storage container for sensor electrode 5 Gas inlet to the measuring cell ...

Страница 37: ... is connected to the connector at the terminal of the sulfuric acid container using a banjo bolt with conical nipple The other end of the gas transfer line is connected to the auto protection assembly in the basic device Fig 31 Sulfuric acid container with outlet in the chlorine module 1 Safety attachment 2 Sulfuric acid container with outlet 3 Hose to the measuring gas line 4 Drain cock for the s...

Страница 38: ... sensitive and high concentration Fig 33 Introducing gas to the measuring cell multi purpose combustion tube 3 6 Autosampler sample introduction systems The following autosamplers and sample introduction systems are available for the multi X 2500 Autosampler autoX 36 autoX 36d Autosampler autoX 112 Automatic boat feeder ABD Manual boat feeder MBD Auto injector ...

Страница 39: ...ethod autoX 36d Autosampler with ejection function for direct dosing of activated carbon from a maximum of 36 columns 18 x 6 mm It can be employed for samples which were enriched using the column method Both autosamplers are connected to the multi X 2500 by means of the interface cable The multiWin control software automatically detects autosamplers and sample racks and controls the introduction o...

Страница 40: ...autoX 36 stacked on the multi X 2500 1 Autosampler autoX 36 2 Cover with ejection function 3 Interface cable 4 Mount in the cutout of the multi X 2500 Fig 36 autoX 36d with ejection position Fig 37 Sample racks 1 Sample rack for autoX 36d 2 Sample rack for autoX 36 ...

Страница 41: ...e fastening screws on the combustion furnace by its bracket MBD and combustion tube are connected using a connection piece which is screwed onto the combustion tube It ensures that the connection is gas tight The MBD is connected to the interface in the device interior 3 in Fig 5 on page 20 using the connection cable The MBD is then identified by the multiWin software Argon is used as carrier and ...

Страница 42: ...o the oxygen connection it has a pneumatic unit which is used to move the clamping device for the sample downward The pre combustion adapter is connected to the multi X 2500 via the pneumatic box It is then possible to use the multiWin control software to determine for how long the sample is supposed to be pre dried in the upper part of the combustion tube clamped in between the glass tube and the...

Страница 43: ...ctions and assemblies of the device may corrode Free from draft air do not install the device close to windows or doors Away from electromagnetic sources of interference No direct sunlight and away from radiant heaters The front door and air vents must not be obstructed by other equipment or furnishings Keep a safety distance of at least 20 cm from the rear of the device to other equipment or wall...

Страница 44: ... customer service Required gases see section Technical data p 122 ff 4 4 Space requirement and device layout The space requirements are based on the system modules required for the measuring task In addition to that the setup requires space for a PC a monitor and a printer Device Dimensions width x height x depth in cm Basic device multi X 2500 51 x 47 x 56 Cl module or TOC module each 30 x 47 x 5...

Страница 45: ...multi X 2500 Installation and commissioning 45 Fig 41 Vertical operating mode with autoX 112 Fig 42 Horizontal operating mode with ABD and autoX 112 ...

Страница 46: ...vice department of Analytik Jena AG or authorized and trained specialist personnel Check when unpacking the device for completeness and soundness of the delivery in accordance with the packing list included After assembly the customer service tests the functionality of the multi X 2500 and other system components and documents the test NOTICE Always switch off all components of the multi X 2500 be...

Страница 47: ...ust vent 4 Connect the provided gas hose to the oxygen supply of the laboratory and the gas connection O2 IN on the rear of the device Optional versions AOX horizontal EOX POX TX 5 Connect the exhaust air hose to the outlet waste of the chlorine module 4 Connect the hose to an extraction system or place it into an exhaust vent 6 Connect the provided gas hose to the oxygen supply of the laboratory ...

Страница 48: ...al system components The proper connection of additional system components to the multi X 2500 basic device is described in the user manual of the respective system component Sample feeder autoX 112 Auto injector Automatic boat feeder ABD Manual boat feeder MBD TOC module ...

Страница 49: ...and analysis software Log in with user name and password 4 Initialize the analysis system by clicking on INITIALIZE ANALYZER The initialization and automatic detection of all connected components will be executed After logging in the components are initialized and polled The current values are displayed in the status window Furnace temperature The preheating time is approximately 30 to 40 minutes ...

Страница 50: ...c acid has been drained or the device has cooled down A vacuum may build up when the device cools down which may draw sulfuric acid into the gas transfer line As long as the gas supply is open the argon safety bypass on the auto protection assembly prevents this from happening 1 Exit the multiWin control and analysis software 2 Remove the gas transfer line from the sulfuric acid container in the c...

Страница 51: ...id container Changing the sulfuric acid and cleaning the sulfuric acid container with outlet p 101 2 Disconnect the gas transfer line inside the basic device from the auto protection assembly and remove the connector of the heating cable from the socket 3 Carefully remove the gas transfer line from the basic device and check it for contamination with sulfuric acid 4 If necessary clean the gas tran...

Страница 52: ...ation from waters Please observe the following The AOX method can be used to determine AOX contents of more than 10 µg l directly The DOC content should be smaller than 100 mg l Otherwise the sample must be diluted especially if it contains alcohols aromatics or carboxylic acids The content of inorganic chloride or bromide should be smaller than 1 g l Otherwise the sample must be diluted or replac...

Страница 53: ...an they produce with the column method 1 Add 100 ml of the sample 5 ml of nitrate stock solution and 50 mg AOX carbon to a 250 ml Erlenmeyer flask Use a plug to seal the flask The AJ filling device is recommended for metering the AOX carbon 2 Shake the suspension for 1 hour 3 Use a membrane filter apparatus to separate water activated carbon or water activated carbon sludge with a chloride free po...

Страница 54: ...shake the mixture for 1 hour After that the samples are filtered using a membrane filtration apparatus or the AFU 3 washed with nitrate wash solution and combusted 6 2 AOX determination in vertical operating mode recommended Sample preparation Column and batch method Operating mode Vertical Measuring cell sensitive Measuring range 1 to 100 µg Cl Electrolyte volume 15 to 20 ml Combustion tube Open ...

Страница 55: ...erspiration cause crystallizations in the quartz glass when heating the combustion furnace which reduce the service life of the combustion tube Do not touch the combustion tube with your hands Wear protective gloves If necessary clean the combustion tube externally before installing it in the combustion furnace e g by wiping it with moist cellulose 1 Exit the multiWin control software Wait until t...

Страница 56: ...arrow Only then the gas will be able to flow freely The open combustion tube is mounted and can be connected to the sulfuric acid container 8 Mount the heat bridge in the cutout for the furnace above the gas outlet of the combustion tube Insert the sulfuric acid container vertically WARNING Concentrated sulfuric acid can cause severe chemical burns Wear appropriate protective clothing when working...

Страница 57: ... combustion furnace 5 Connect the sulfuric acid container to the open combustion tube using the forked clamp 3 6 Connect the measuring gas hose 4 via the spherical joint adapter to the sulfuric acid container Secure the connection with a forked clamp 7 If not already done route the measuring gas hose through the holes at the top of the basic device s and the chlorine module s side panels 8 Put the...

Страница 58: ...rage container for the combined electrode 4 into the bracket in the door of the chlorine module 5 Connect the gas outlet of the measuring cell 5 via the olive tip suction adapter and hose no 5 to the upper end of the adsorption tube 6 Connect the lower end of the adsorption tube to the intake pump using hose no 4 7 Attach the measuring gas hose to the connection of the combined electrode 6 8 Elect...

Страница 59: ...d nitric acid 4 g of gelatin 1 0 g of thymol 0 3 g of thymol blue 500 ml of methanol The electrolyte solution for the measuring cells sensitive and high concentration is prepared as follows 1 Solution A Fill 500 ml of water into a 1000 ml volumetric flask add 4 ml of HNO3 conc carefully add 200 ml of acidic acid and top up with water up to the marking 2 Solution B1 Mix 4 g of gelatin in a beaker w...

Страница 60: ...ensitive 200 µl of a 0 01 N HCl solution Measuring cell high concentration 200 µl of a 0 1 N HCl solution 3 Start the end point routine immediately after metering by clicking OK 4 The status END POINT ROUTINE is displayed during the process in the window STATUS ANALYZER After the end point routine the status STAND BY TITRATION and the current indicator value are displayed in the window STATUS ANAL...

Страница 61: ...6 Start the control and analysis software multiWin and log in with user name and password 7 Initialize the analysis system by clicking on INITIALIZE ANALYZER The initialization and automatic detection of all connected components will be executed In the window DEVICE STATUS any components not yet ready for operation will be shown in red The time it takes to preheat the furnace to 950 C is about 30 ...

Страница 62: ...ifications in the safety data sheet 1 Connect the autosampler to the sampler connection on the rear panel of the multi X 2500 using the interface cable 2 Fill the sulfuric acid container vertical with fresh sulfuric acid every day If necessary remove any used quartz containers from the open combustion tube 3 When using the autosampler autoX 36d with ejection function Use tweezers to place the quar...

Страница 63: ...up phase it is not possible to start a measurement If the analyzer is still not ready for measurements after about 40 min carry out a fault analysis in accordance with the notes in chapter Fault removal on page 106 11 Carry out the end point routine for the measuring cell 12 If necessary test the measuring cell using a direct method 13 When prompted by the control and analysis software multiWin pl...

Страница 64: ... open the front doors 3 Replace the oxygen sluice on the open combustion tube by the pre combustion adapter 4 Connect the angled adapter 1 with the oxygen hose hose no 3 to the adapter 5 Connect the hose of the pneumatic unit 2 to hose no 20 in the multi X 2500 Hose no 20 is attached to a bracket at the top of the housing of the multi X 2500 6 Reinsert the top cover Close the doors 7 Connect the i...

Страница 65: ...inserted into a quartz glass boats The quartz glass boat is then introduced into the combustion tube using the manual boat feeder MBD or the automatic boat feeder ABD For large sample series it is possible to combine the ABD with the autosampler autoX 112 Installation and commissioning of the ABD and the autoX 112 are described in the respective devices user manuals 6 3 1 Preparing the analyzer op...

Страница 66: ...the auto protection assembly to the combustion furnace 4 Screw hose no 8 1 into the connection 5 Plug in hose no 11 2 Push down the ring of the plug in connector to do this 6 Screw the gas transfer line 3 into the connection at the side 7 Insert the electrical connections for the auto protection assembly 4 and for the gas transfer line 5 into the terminals 8 Route the gas transfer line through the...

Страница 67: ... tube externally before installing it in the combustion furnace e g by wiping it with moist cellulose NOTICE Closing the pneumatic seal when the combustion tube has not been inserted into the furnace may destroy the auto protection assembly Only move the toggle switch down if a combustion tube has been inserted 1 Open the service flaps on the right hand side of the basic device 2 Insert the multi ...

Страница 68: ... safety data sheet NOTICE Risk of damaging the intake pump of the chlorine module Make sure to properly connect the gas supply in the measuring cell when using the multi purpose combustion tube Never connect the measuring cell to the intake pump via the olive tip suction adapter and the hose Otherwise electrolyte will be drawn into the pump unit The hose of the transfer line is connected to the co...

Страница 69: ...ic acid container Make sure that the conical nipple tightly seals the sulfuric acid container 4 Screw the connector 3 onto the sulfuric acid container 5 Pass the transfer line 1 through the banjo bolt 2 to connect it with the connector Make sure that the conical nipple tightly seals the banjo bolt 6 Place the Petri dish 5 and the beaker 6 under the sulfuric acid container ...

Страница 70: ...aging the intake pump of the chlorine module Make sure to properly connect the gas supply in the measuring cell when using the multi purpose combustion tube Never connect the measuring cell to the intake pump via the olive tip suction adapter and the hose Otherwise electrolyte will be drawn into the pump unit The measuring cells sensitive and high concentration are inserted to the chlorine module ...

Страница 71: ...e tip suction adapter to the exhaust air hose in the chlorine module 6 Connecting the combined electrode and the measuring cell at the inside of the rear panel of the chlorine module Connection combined electrode 1 Connection measuring cell 2 6 3 2 Preparing the measuring cell The preparation of the measuring cell for daily measurements includes the following steps Preparation of the electrolyte s...

Страница 72: ...the intake pump via the olive tip suction adapter and the hose Otherwise electrolyte will be drawn into the pump unit 3 The analyzer and the chlorine module are switched on The devices are booted The status LEDs on the front panel lights up in green after approximately 30 seconds 4 Open the gas supply and set the primary pressure to 4 to 6 bar 5 Switch on the PC 6 Start the control and analysis so...

Страница 73: ...nd METHOD METHOD ACTIVATE 13 Starting the measurement Select START START ANALYSIS Select an analysis group or create a new one Create an analysis sequence Enter the sample ID for all samples in the field NAME Confirm the entry with OK Click the START MEASUREMENT button The prepared analysis sequence is processed For manual sample introduction follow the prompts in the control and analysis software...

Страница 74: ...cases The transformed hydrogen halides are determined in the measuring cell high sensitive or sensitive depending on the concentration of the sample The use of the measuring cell high sensitive is recommended for very low EOX contents For the EOX determination the extracts are introduced directly to the combustion tube via the injection port For this purpose a screw cap with septum is attached to ...

Страница 75: ...ombustion tube must not be mixed up CAUTION Risk of burns Only install the combustion tube in the cold state NOTICE Alkaline salts hand perspiration cause crystallizations in the quartz glass when heating the combustion furnace which reduce the service life of the combustion tube Where possible do not touch the combustions tube with your hands during installation Wear protective gloves If necessar...

Страница 76: ... in the flame sensor 3 to the connection if used 7 Screw a screw cap with septum to the combustion tube 8 Close the pneumatic seal to the auto protection assembly To do this move the toggle switch 1 down The combustion tube is now locked in the auto protection assembly 9 In vertical operating mode put the cover at the top back into place 10 Connect a sample introduction module For the EOX determin...

Страница 77: ...asuring cell with electrolyte Preparing the measuring cell p 78 3 Insert the storage container for the sensor electrode into the bracket in the door of the chlorine module Fill the storage container with approximately 2 to 3 ml of internal electrolyte 4 Insert the sensor electrode with pre amplifier 1 into the Sen opening of the measuring cell 5 Insert the silver electrode 2 into the Ag opening 6 ...

Страница 78: ...measuring cells sensitive and high concentration Measurements with the measuring cell high sensitive require an electrolyte solution In addition to that an internal electrolyte for the sensor electrode must be prepared which is also used for storing the electrode WARNING 100 acetic acid glacial acetic acid can cause severe chemical burns Wear the appropriate protective clothing when preparing the ...

Страница 79: ...d between two measurements of a multiple determination The status END POINT ROUTINE is displayed during the process in the window STATUS ANALYZER Indicator value greater than 10000 Silver ions are automatically produced The value set for the operating point of the electrolyte is 3000 Indicator value less than 1000 The software prompts the user to add a dose of 10 mg l of HCl to the measuring cell ...

Страница 80: ...Otherwise electrolyte could get drawn into the pump 3 The analyzer and the chlorine module are switched on The devices are booted The status LEDs on the front panel lights up in green after approximately 30 seconds 4 Open the gas supply and set the primary pressure to 4 to 6 bar 5 Switch on the PC 6 Start the control and analysis software multiWin and log in with user name and password 7 Initializ...

Страница 81: ...e menu command METHOD METHOD ACTIVATE 13 Starting the measurement Select START START ANALYSIS Select an analysis group or create a new one Create an analysis sequence Enter the sample ID for all samples in the field NAME Confirm the entry with OK Click the START MEASUREMENT button The prepared analysis sequence is processed For manual sample introduction follow the prompts in the control and analy...

Страница 82: ...ered to the combustion tube using µl syringes The samples are combusted in an argon oxygen stream without any further sample preparation During this process organic halogenated compounds are transformed into hydrogen halides Their mass concentration is determined as chloride Depending on the sample matrix the TX determination is carried out in horizontal operating mode or vertical operating mode I...

Страница 83: ...en stream During this process they are transformed into hydrogen halides whose mass concentration is determined as chloride The analyzer is operated in its default configuration in vertical operating mode with open combustion tube and measuring cell sensitive Refer to chapter AOX determination in vertical operating mode recommended on page 54 for information on the preparation of the analyzer and ...

Страница 84: ...ce the top cover on top of the analyzer 3 Preparing the measuring cell Fill the measuring cell with fresh electrolyte solution every day Measuring cell sensitive 15 to 20 ml Insert the magnetic stirring rod into the measuring cell Attach the cover and tighten it using the three knurled head screw Insert the combined electrode and connect it electrically Electrically connect the measuring cell Conn...

Страница 85: ...uice to the POX sluice CAUTION Risk of burns when touching the oxygen sluice and the combustion tube Wear protective gloves Remove the top cover Pull the angled adapter off the oxygen sluice Remove the oxygen sluice Attach the POX sluice to the top of the combustion tube Connect the oxygen hose 1 hose no 3 to the POX sluice Connect the measuring gas hose 2 hose from the outlet to the POX cylinder ...

Страница 86: ...configured times 15 Activate the new method or an already existing method using the menu command METHOD METHOD ACTIVATE 16 Starting the measurement Select START START ANALYSIS Select an analysis group or create a new one Create an analysis sequence Enter the sample ID for all samples in the field NAME Confirm the entry with OK Click the START MEASUREMENT button The prepared analysis sequence is pr...

Страница 87: ...cracks and damage Monthly Check inspection port with septum for tightness replace septum if using the multi purpose combustion tube Daily as required Sulfuric acid container Replace sulfuric acid As required at least once per day Clean and dry the sulfuric acid container Weekly For trace analysis with measuring cell high sensitive each time the sulfuric acid is changed otherwise the analytic perfo...

Страница 88: ...swapping the gas connections Always connect the gas lines correctly and set the required gas pressures The gas inlets Ar and O2 on the rear of the multi X 2500 are equipped with a particle filter The particle filter must be replaced once the process gases can no longer be set to the target value check for messages in the software and potential leaks within the system have been excluded 1 Switch of...

Страница 89: ...i X 2500 and the chlorine module and switch on the devices using the mains switch The multi X 2500 is ready for operation again 10 3 Maintenance activities standard version 10 3 1 Removing and cleaning the open combustion tube WARNING Concentrated sulfuric acid can cause severe chemical burns Wear protective clothing when working at the sulfuric acid container Observe all specifications in the saf...

Страница 90: ...power outlet Cut the gas supply 3 Remove the top cover or the multi X 2500 or the sample introduction module and open the front doors 4 Detach the connection hose and the spherical joint 1 from the sulfuric acid container vertical 5 Detach the forked clamp 2 between the sulfuric acid container and the combustion tube 6 Carefully remove the sulfuric acid container from the drip tray and empty it Ob...

Страница 91: ...he sulfuric acid must be replaced once per day High sample throughput may require more frequent replacement 1 Exit the multiWin control software and allow the analyzer to cool down 2 Switch off the multi X 2500 and the chlorine module and pull the mains plugs from the power outlet Cut the gas supply 3 Remove the top cover or the sample introduction module and open the front doors 4 Detach the conn...

Страница 92: ...he two connectors to the filled adsorption tube in the chlorine module 9 Press the adsorption tube into its mount NOTICE Do not twist or kink the hoses 10 3 4 Servicing the measuring cell Since the continuous introduction of hot reaction gases during operation causes electrolyte components to evaporate it is recommended to change the electrolyte solution once per day 1 Remove the used electrolyte ...

Страница 93: ...tion one day to the next Store the combined electrode in fresh electrolyte solution For decommissioning over several days Carefully rinse the combined electrode with ethanol and subsequently rinse it with ultrapure water Wipe the combined electrode with cellulose and store it in dry condition 10 4 Maintenance activities optional version 10 4 1 Checking the settings of the gas flows 1 Switch on the...

Страница 94: ...and the chlorine module 2 Drain the entire sulfuric acid from the sulfuric acid container with outlet in the chlorine module Clean and dry the sulfuric acid container Changing the sulfuric acid and cleaning the sulfuric acid container with outlet p 101 NOTICE Always clean and dry the sulfuric acid container Check the hose system for deposits of acid in form of small drips If required clean the hos...

Страница 95: ...ate is not registered The bypass flow rate is at approx 15 ml min It may however vary between 10 and 25 ml min This value must be considered when measuring the flow rate 8 Insert the disposable filter in between the hoses for a second measurement and repeat the reading of the current gas flow rate The filter serves as a small resistance in the gas flow 9 If the gas flow determined during the 2nd m...

Страница 96: ...rom the sulfuric acid container with outlet in the chlorine module 2 Exit the multiWin software and allow the analyzer to cool down Use the mains switch to switch off the multi X 2500 and the chlorine module and cut the gas supply 3 If not already done tilt the combustion furnace into horizontal position 4 Open the pneumatic seal on the auto protection assembly To do this move the toggle switch 1 ...

Страница 97: ...mbly must be checked every three months Proceed as follows 1 Remove the auto protection assembly 2 Check the filter for carbonization soiling or cracks through visual inspection If the filter is OK re install the auto protection assembly If the filter needs replacing follow the remaining instructions 3 Unscrew the 4 screws attaching the pneumatic seal to the auto protection assembly 4 Remove the p...

Страница 98: ...embly is ready for operation again Replacing the pneumatic seal 1 Remove the auto protection assembly 2 Unscrew the 4 screws attaching the pneumatic seal to the auto protection assembly 3 Remove the housing with the pneumatic seal from the auto protection assembly 4 Use an Allen wrench to unscrew the connection bushing for hose no 11 from the seal housing To do this insert the Allen key into the c...

Страница 99: ...FE disk b into the housing c 11 Place the pneumatic seal a into the housing The hole in the ring must align with the hole in the housing 12 Use the Allen wrench to tighten the connection bushing for hose no 11 see item 4 13 Place a second PTFE disk onto the intermediate ring above the filter 14 Place the pneumatic seal onto the auto protection assembly and attach it with 4 screws The auto protecti...

Страница 100: ...nace e g by wiping it with moist cellulose NOTICE Closing the seal when the combustion tube has not been inserted into the furnace may destroy the pneumatic seal of the auto protection assembly Only move the toggle switch down if a combustion tube has been inserted Alternatively we recommend to cut the gas supply during maintenance 1 Disconnect the gas transfer line from the sulfuric acid containe...

Страница 101: ...multi purpose combustion tube S 67 for information on the reinstallation of the multi purpose combustion tube 10 4 5 Changing the sulfuric acid and cleaning the sulfuric acid container with outlet WARNING Concentrated sulfuric acid can cause severe chemical burns Wear protective clothing when working at the sulfuric acid container Observe all specifications in the safety data sheet The sulfuric ac...

Страница 102: ...m the gas inlet tube When using the measuring cells sensitive and high concentration from the combined electrode 3 Detach the safety clips and remove the safety attachment 4 from the sulfuric acid container WARNING There may be residual sulfuric acid on the ground surface of the sulfuric acid container 4 Open the drain cock and let the entire sulfuric acid flow into the beaker 5 Once the sulfuric ...

Страница 103: ...leaning the acid container 1 Drain the sulfuric acid container with outlet as described above 2 Rinse the sulfuric acid container with distilled water to avoid any contact with the acid when handling the container afterwards 3 Remove the sulfuric acid container from the chlorine module 4 Detach the banjo bolt 2 and disconnect the gas transfer line 1 from the connector 3 5 Unscrew the connector 3 f...

Страница 104: ...l high sensitive only top up electrolyte 1 Remove the used electrolyte 2 Rinse the measuring cell and the magnetic stirring rod with distilled water and with ethanol 3 Then carefully wipe out the measuring cell and wipe the magnetic stirring rod with cellulose to remove any silver chloride deposits 4 Top up or fill the measuring cell with fresh electrolyte Measuring cell high sensitive approx 65 m...

Страница 105: ...d the filling level should remain visible above the cover of the measuring cell If required use the refilling port to top up with 0 6 mol l Na2SO4 solution or replace the solution The solution should preferably be refilled at the end of a working day or the end of a working week since the electrode should be allowed a stabilization time of 2 to 24 hours depending on its degree of aging Top up at l...

Страница 106: ...lytik Jena if the fault cannot be remedied This also applies for the repeated occurrence of individual faults The zip file that was created must be sent by email to the customer service department at Analytik Jena for the fault diagnosis 11 1 Troubleshooting according to software messages NOTICE Unsuitable USB cables or impermissible extensions often cause problems in the communication between the...

Страница 107: ...art operating system PC Restart firmware basic device Restart multiWin 12 Signal echo received check interface selection Cause Remedy Incorrect port selected Check port selection 14 Data transfer interrupted Cause Remedy No data transfer for 10 s Initialize 17 Wrong interface protocol ID Cause Remedy Fault after update program versions of firmware multiWin don t match Update required 20 Timeout In...

Страница 108: ... structure Cause Remedy Error in communication with chlorine module Acknowledge message Switch chlorine module on off Initialize 132 Cl sensor Indication error Cause Remedy Indicator value after titration start out of range measurement cannot start Acknowledge message Initialize Execution of the end point routine Check status of measuring cell via SYSTEM COMPONENT TEST CHLORINE 133 Cl sensor wrong...

Страница 109: ...essary during an overpressure in the system Never switch off a device that is subject to overpressure Do not introduce any samples Do not close multiWin Do not switch off basic device and module Do not switch off the gas supply Manually ventilate device via chlorine module Manual ventilation WARNING Concentrated sulfuric acid Wear safety clothing Detach hose connection to measuring cell Detach gas...

Страница 110: ...e hindrance if required Replace rack Initialize 226 Sampler runtime exceeded Cause Remedy Message from autoX 112 sampler saying that the movement is completed takes too long autoX 112 defective Record log files Report to customer service 230 ABD no connection Cause Remedy Communication error after ABD was detected during initialization Acknowledge message Initialize 232 Flame sensor error Cause Re...

Страница 111: ...alize 11 2 Equipment faults and analytical problems 11 2 1 General notes 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 measuring results which seem to be implausible analytical problems or they are clearly indicated by the equipment technology If the suggested solutions are not successful info...

Страница 112: ...tion transfer line to the auto protection assembly leaking In the horizontal operating mode transition coupling tube to ABD leaking Check connection and ensure correct fit at the connection points Check argon supply open the pneumatic seal with the toggle switch Check position of the septum insert new septum if necessary Check connection Check sealing of the coupling element check alignment betwee...

Страница 113: ...rations in the method Check calibration repeat if required Close liquid samples Check the sampler routine for solid samples Particularly for solids set a post combustion time of 120 s in the method Clean or replace sooted parts Carryover Cause Solution Inadequate rinsing of the sample introduction components Combustion tube insufficiently rinsed for EOX determinations Contamination within the inje...

Страница 114: ...e switch to switch off the basic device and the chlorine module respectively 3 Cut the gas supply 4 Disconnect the mains plugs from the power outlets 5 Detach all connections on the rear panel of the basic device and the rear panel of the chlorine module Gas connectors Serial connection cable Mains cable Exhaust air hose 1 Detach the hose connection to the measuring cell and the connection to the ...

Страница 115: ... 2500 is operated with the optional multi purpose combustion tube proceed as follows to prepare the device for transport 1 Exit the multiWin control and analysis software 2 Remove the gas transfer line from the sulfuric acid container with outlet in the chlorine module and drain the sulfuric acid from the sulfuric acid container Changing the sulfuric acid and cleaning the sulfuric acid container w...

Страница 116: ...105 4 Remove the measuring cell and rinse it WARNING The electrolyte solution of the measuring cell high sensitive contains concentrated acetic acid Be careful when emptying the measuring cell 5 Attach the extraction hose to the chlorine module using adhesive tape 12 3 Removing and installing the combustion furnace 12 3 1 Removing the combustion furnace WARNING Danger of electric shock Before remo...

Страница 117: ...ate connection 7 Detach the connectors from the slots Connector of the flame sensor 1 Connector of the combustion furnace 2 Connector of the thermocouple 3 To do this slightly lift the gray lever on the connector of the furnace 2 see circle 8 Tilt the combustion furnace into horizontal position 9 If required remove the auto protection assembly from the combustion furnace Servicing the auto protect...

Страница 118: ...the combustion furnace switch off the multi X 2500 using the mains switch and disconnect the mains plug from the power outlet 1 Make sure that the multi X 2500 is not connected to the mains 2 Remove the top cover Open the doors of the multi X 2500 and remove them from the device 3 Insert the combustion furnace horizontally into the multi X 2500 4 Tilt the combustion furnace into vertical position ...

Страница 119: ...he cables for the flame sensor and the thermocouple into the hose clamps 7 Tilt the combustion furnace into horizontal position 8 If required install the auto protection assembly Installing the auto protection assembly p 65 9 Install the combustion tube Inserting the open combustion tube p 55 or Inserting the multi purpose combustion tube p 67 10 Place the top cover on top of the device and reinse...

Страница 120: ... must be free from halogens and hydrocarbons low in dust and free from aggressive vapors If the multi X 2500 is not installed immediately after delivery or not operated over an extended period of time its individual components must be stored in their original packaging A suitable desiccant must be added to the packaging and or the devices to prevent damage from moisture Refer to Technical data on ...

Страница 121: ...rbon used for the adsorption of acetic acid vapor must be disposed of in accordance with legal regulations The sensor electrodes contain mercury At the end of their useful life the sensor electrodes must be disposed of in accordance with the applicable regulations regarding toxic waste Mercury must not enter the sewerage system surface water ground water or the soil The combined electrodes contain...

Страница 122: ...l as an option EOX POX TOC AOX Direct injection of the loaded activated carbon in the quartz container or ejection of the loaded activated carbon from the container in the open combustion tube EOX Direct injection of the extract into the multi purpose combustion tube via injection port with septum POX After purging and transfer in carrier gas stream via special sluice for the open combustion tube ...

Страница 123: ...n 4 5 or better Primary pressure 4 to 6 bar Gas consumption approx 10 l h Power supply 110 to 240 V AC 50 60 Hz Fuse for basic device T 10 A H 2x Fuse for chlorine module T 4 0 A H 2x Only use original fuses from Analytik Jena Typical average power consumption of the basic device 1000 VA Typical average power consumption of the Cl module 100 VA PC interface USB Temperature 20 to 35 C Humidity 90 m...

Страница 124: ...14 35 EU and 2014 30 EU The device leaves the factory in a sound condition as far as technical safety is concerned To maintain this condition and to ensure safe operation the operator must strictly observe the safety and operating instructions contained in this operating manual For accessories which have also been supplied and system components from other manufacturers their operating instructions...

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