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Sulfur analysis with the Coulometric Sulfur Module

multi EA 5000

Figure 53Coulometric sulfur detector with measuring cell (without door)

1 Indicator electrodes connection

2 Indicator electrode (black)

3 Gas inlet

4 Measuring cell

5 Port for manual dosing

6 Anode (yellow)

7 Cathode (red)

8 Generator electrodes connection

Summary of Contents for Analytik Jena multi EA 5000

Page 1: ...Operating Manual multi EA 5000 C N S X Analyzer...

Page 2: ...se Stra e 1 07745 Jena Germany Phone 49 3641 77 7407 Fax 49 3641 77 9279 Email service analytik jena com General Information http www analytik jena com Documentation Number 11 0203 005 23 Edition 02 2...

Page 3: ...and repair 15 4 Function and design 16 4 1 multi EA 5000 basic module 16 4 1 1 Principle of operation 16 4 1 2 Design of the basic module 18 4 2 Sampling modules 29 4 2 1 Auto injector 29 4 2 2 Manua...

Page 4: ...4 10 1 Function and design 74 10 1 1 Function and measuring principle 74 10 1 2 Design 74 10 1 3 Connection 80 10 2 Installation 81 10 3 Operation 83 10 3 1 Preparing the measuring cell 83 10 3 2 Oper...

Page 5: ...ntenance and care 127 14 1 Overview of maintenance work 127 14 2 Maintenance of the multi purpose combustion tube 129 14 2 1 Removing the combustion tube 130 14 2 2 Cleaning the combustion tube 131 14...

Page 6: ...TIC reactor 165 14 14 5 Replacing the pump hose of the condensate pump 167 14 14 6 Cleaning the condensation coil 168 14 14 7 Replacing the catalyst in the TOC combustion tube 169 15 Transport and sto...

Page 7: ...are indicated by a warning triangle and a signal word The type source and consequences of the hazard are stated together with notes on preventing the hazard Elements of the control and analysis progr...

Page 8: ...te water EC OC determination in particulate emissions e g air quality control three way catalytic converter research AOX and EOX for water sludge and soil via the column or batch method Unsuitable sam...

Page 9: ...Fluo rine is not detected AOX Adsorbable organically bound halogens The AOX parameter is the sum of organically bound halogens chlorine bromide iodine adsorbed under defined conditions pH 2 with HNO3...

Page 10: ...aning Comment Warning against dan gerous electrical volt age In the device interior on the electronics cover Warning against electrical voltage Be fore opening the electronics the device must be disco...

Page 11: ...ected system components We recom mend training by qualified employees of Analytik Jena AG or its representatives In addition to the safety instructions in this user manual the general applicable safet...

Page 12: ...uipment must be checked regularly Any defects must be corrected as soon as they occur Protective and safety equipment must never be removed modified or switched off during operation Free access to the...

Page 13: ...e Cl module or when searching for a gas leak in the measuring gas connection between the basic module and the Cl module Work on the electronics may only be carried out by the customer service of Analy...

Page 14: ...e solution in the high sensitive measuring cell has a high concentration of acetic acid To decontaminate rinse out the sulfuric acid container with its safety attachment and the measuring cell with di...

Page 15: ...ice For this reason only the activi ties described in the user manual in the Maintenance and care chapter may be per formed by the operator Only clean the exterior of the device with a slightly moiste...

Page 16: ...tc multiple times per second 4 1 1 Principle of operation 4 1 1 1 Vertical and horizontal operation Operation is in vertical or horizontal mode depending on the installation position of the furnace De...

Page 17: ...oxygen flow during the second phase This digestion is summed up via the following equations R H O2 CO2 H2O R N O2 NOx CO2 H2O R S O2 SO2 CO2 H2O R X O2 HX CO2 H2O R carbonic substance X F Cl Br I TOC...

Page 18: ...c acid in the Cl module TOC NPOC TIC Condensation through Peltier cooling in the TOC module 4 1 2 Design of the basic module 4 1 2 1 Main components Main components of the basic module The multi EA 50...

Page 19: ...t device 5 Pump connection for N S C mode 6 Combustion furnace 7 Knob for tilting the furnace Horizontal device Furnace in horizontal installation position Opening with maintenance flaps at the right...

Page 20: ...ules Operational LED Figure 4 Basic module with a sampling module and a detection module A green LED is installed on the left door of the basic module After loading the control and analysis software t...

Page 21: ...Interfaces on the rear of the device 1 Gas connectors 3 USB port for PC 2 Power connection power switch 4 Interfaces for detector modules and sampling modules 1 2 3 Figure 6 Power connection power swi...

Page 22: ...for the combustion furnace the flame sensor and the temper ature sensor can be found on the rear interior side of the device The connections are only accessible in the vertical installation position...

Page 23: ...and clos ing the pneumatic seal in the auto protection valve assembly 2 Transfer line heating connection 3 Valve assembly connection 4 1 2 3 Gas supply hose diagrams Hose diagrams The connection betw...

Page 24: ...O2 ABD Filter 2 3 4 5 6 7 8 1 9 10 11 12 13 14 15 16 ABD Gas box Combustion furnace Rotary bearing Rotary bearing Coupling Exhaust Membrane dryer Filter Pump to the N S C detector N S C outlet MFM Cl...

Page 25: ...1 2 5 6 7 9 10 14 15 13 ABD 3 4 8 11 12 Membrane dryer Rotary bearing Rotary bearing Combustion furnace Coupling Gas box Filter Exhaust Pump to the N S C detector N S C outlet MFM Cl system tightness...

Page 26: ...luded con nection hoses AD 6 mm ID 4 mm 1 2 3 4 5 Figure 12Gas connections at the rear of the device 1 Argon gas inlet Ar 2 Gas outlet to the N S C module 3 Purge gas outlet of the membrane dryer with...

Page 27: ...ve assem bly hose 11 4 dryer dry gas flow oxygen for the membrane dryer hose 12 5 bypass argon connection for the safety purging safety bypass of the chlorine branch hose 8 Connections on the combusti...

Page 28: ...o the required operating mode quickly via the tilt device Figure 15 Combustion furnace in the vertical and horizontal operating mode A multi purpose combustion tube used for all standard applications...

Page 29: ...ntainer via a transfer line To determine TOC NPOC TIC via condensation with Peltier cooling in the TOC module 4 2 Sampling modules 4 2 1 Auto injector There are two types of auto injector The classic...

Page 30: ...sfer speed and thus the introduction of the sam ple into the combustion zone The MBD may only be used in horizontal operation mode for inert non reactive solids e g SiO2 and AOX samples The MBD may no...

Page 31: ...te vicinity of the device and its system components These could corrode the device connections and modules Free from draft air do not install the device close to windows or doors Away from electromagn...

Page 32: ...ght of the basic device or on top of it 1 detection module to the left of the basic device Several modules may also be placed in a row Component Width x Height x Depth mm Mass kg Arrangement Basic mod...

Page 33: ...he basic module Autoinjector AI EA 150 x 270 x 240 mm 1 5 kg On the basic module GSS LPG combi module GSS module or LPG module 2 0 300 x 800 x 550 mm 11 kg 12 kg To the right of the basic module or AB...

Page 34: ...Installation and commissioning multi EA 5000 34 Figure 19Space required for the basic device and modules horizontal operation...

Page 35: ...he analysis system after installa tion and documents the test Installing the basic module Carefully remove the basic module and its components from the transport packaging Do not damage the transport...

Page 36: ...ct the power plug to a grounded power outlet Connect the supplied connection hoses to the pressure reducers of the gas supply and the the O2 and Ar gas connections on the rear of the device media conn...

Page 37: ...sor in automatic or automatic plus mode or an Autoinjector To add samples of flammable substances do not use the ABD in parameter mode or only use it with program parameters designed and tested for it...

Page 38: ...mple Furnace installation po sition and sampling Comment TS TN TX TC in Organic solids e g wax polymer Horizontal for ABD ABD with MMS ABD with flame sensor For trace analysis Use 1 quartz glass boat...

Page 39: ...l GSS module recom mended Gas pressurized Horizontal or vertical for GSS LPG combi module GSS module with GSS adapterbox with ABD horizontal LPG Horizontal or vertical GSS LPG combi module LPG module...

Page 40: ...e electronics can overheat and become damaged due to lack of cooling Only switch off the basic module after a cooling time of 1 h Switch off the basic modules and its modules as follows Exit the multi...

Page 41: ...protection valve assembly in the basic module Remove the heating cable plug from its socket Carefully remove the gas transfer line and check it for contamination with sulfuric acid If necessary clean...

Page 42: ...valve assembly Plug the heating cable plug into its socket Route the gas transfer line through the wall of the basic module top the detection module Connect the gas transfer line to the sulfuric acid...

Page 43: ...tted is proportional to the NO2 concentration This allows measurement of the concentration via light NO is the only substance involved in the reaction which means that this method is very selective an...

Page 44: ...of excess ozone O3 Diaphragm pump Conveyance of the measuring gas through the detector Differential pressure sensor Regulation of the pressure compensa tion between the variable measuring gas flow an...

Page 45: ...e located beneath it Communication with the basic module is performed via a 9 pin interface cable The in terface of the rear of the detector is marked with N CLD The gas for producing ozone is connect...

Page 46: ...pt the function of other optical detection modules or lead to serious errors Always connect the detection module as the last in any series of the detectors Install the detection module as the last in...

Page 47: ...e detection module N CLD on the rear of the basic module Connect the measuring gas hose of the basic module to the sample in gas inlet on the rear of the module Connect an approx 50 cm long hose to th...

Page 48: ...possible Open the gas supply and set the required gas pressure Switch on the PC Start the control and analysis software and login with your username and password Initialize the analysis system by cli...

Page 49: ...there via microcoulometric titration Hydrogen flouride HF is not determined In the first step hydrogen chloride HCl dissolves in the electrolyte and dissociates to hydrogen and chloride ions H Cl In t...

Page 50: ...is switched on the magnetic stirring rod in the measuring cell starts moving The preset cell temperature is 18 C and can be modi fied as a method parameter in the control and analysis software The sen...

Page 51: ...ipped measuring cell 1 Combined electrode 2 Olive for connecting to the exhaust The combined electrode is used for the sensitive and high concentration measuring cells It combines the indicator electr...

Page 52: ...r electrolyte volume It is suitable for a chlorine content of 10 to 1000 g and is recommended in particular for TX determination of highly contaminated waste and of polymer samples with high PVC conte...

Page 53: ...al borehole is intended for an adapter that is connected to the exhaust hose It is used as an exhaust for the acetic acid vapors The small unmarked opening is used for direct injection into the cell T...

Page 54: ...de with salt bridge 7 Measuring cell Sensor electrode The sensor electrode combines the indicator and reference electrodes A 0 6 mol l sodium sulfate solution is used as an internal electrolyte which...

Page 55: ...re applied to the adapter and connected to the exhaust hose One side of the T piece remains open The acetic acid vapors can be drawn out of the detec tion module effectively without the electrolyte so...

Page 56: ...e 1 Platinum electrode with salt bridge complete 2 Salt bridge 3 Platinum electrode with screw on cap and sealing ring Figure 35Silver electrode The storage container for the sensor electrode can be f...

Page 57: ...ul inter face is also located on the rear of the module The gas outlet for connection to the ex haust hose of the laboratory exhaust system is located at the bottom left of the rear panel 1 2 3 4 5 Fi...

Page 58: ...ion with a banjo bolt with a conical nipple The other end of the gas transfer line is con nected to the auto protection valve assembly in the basic device 1 2 3 4 5 6 7 3 5 4 Figure 38Connection of th...

Page 59: ...he Cl module 59 Figure 39Gas infeed tube with PTFE connector In both cases the measuring gas hose is fastened with the aid of a PTFE connector En sure the proper fit of the sealing rings Figure 40Gas...

Page 60: ...nnect the modules to power when they are switched off Place the detection module to the immediate left of the basic module Connect the supplied power cable to the power cable connection on the rear of...

Page 61: ...gas transfer line to the sulfuric acid container Insert the thin hose 3 into the sulfuric acid container Connect the connector 4 to the sulfuric acid container Connect the gas transfer line via the b...

Page 62: ...uring cell with magnetic stirring rod and lid into the de tection module Fill the measuring cell with electrolyte solution Insert the combined electrode into the marked opening of the measuring cell F...

Page 63: ...container with approximately 2 to 3 ml of internal electrolyte Insert the components in the following openings Sensor electrode with pre amplifier 1 Sen opening Silver electrode 2 Ag opening Platinum...

Page 64: ...blue 500 ml methanol Solution A Fill 500 ml of water into a 1000 ml volumetric flask add 4 ml of HNO3 conc care fully add 200 ml of acidic acid and top up with water to the marking Solution B1 Mix 4 g...

Page 65: ...nu item in the Chlorine tab Protecting the combined elec trode Observe the following to protect the combined electrode against unnecessary wear Always add fresh electrolyte to the measuring cell befor...

Page 66: ...ating range When working with a MMS the addition of chloride ions to the measuring cells can be performed automatically if the indicator value goes below the operating range while an analysis sequence...

Page 67: ...ry problems due to leaking acetic acid vapors The electrolyte solution of the high sensitive measuring cells contains high concentra tions of acetic acid Ensure that the exhaust hose is connected to t...

Page 68: ...n daily sensitive measuring cell 15 to 20 ml high concentration measuring cell 120 ml The high sensitive measuring cell Fill the measuring cell daily with electrolyte solution to approx 65 ml Change t...

Page 69: ...R Hydrocarbon residue The detection is performed using the UV fluorescence method Sulfur dioxide SO2 ex cited via UV light emits a characteristic flourescence 220 to 420 nm This flourescence is measur...

Page 70: ...wise the measurement results will be too low Conversely use of cali bration with an active MPO for a method with no MPO can lead to false measurement results that are too high 9 1 3 Connection The equ...

Page 71: ...the basic module and of the detection module Always connect the modules to power when they are switched off Place the detection module to the left of the basic module In the event of a series of dete...

Page 72: ...ogy Install the chemical ozone decomposer on the rear of the module Fasten the two holding clamps with the supplied screws First press the chemical ozone decomposer into the upper holding clamp and th...

Page 73: ...then possible Open the gas supply and set the required gas pressure Switch on the PC Start the control and analysis software and login with your username and password Initialize the analysis system by...

Page 74: ...oxides dissolve in the electrolyte and react with iodine This decreases the cell potential R S O2 SO2 SO3 CO2 H2O 2 H2O SO2 I2 H2SO4 2 HI R Hydrocarbon residue After a specified accumulation time depe...

Page 75: ...5 1 2 3 5 6 7 8 4 Figure 46Coulometric sulfur detector with measuring cell without door 1 Indicator electrodes connection 2 Indicator electrode black 3 Gas inlet 4 Measuring cell 5 Port for manual dos...

Page 76: ...cell The measuring cell is equipped with electrodes for generation and indication The elec trodes are color coded Generation Yellow anode red cathode Indication Black indicator electrodes The measurin...

Page 77: ...manual dosing 4 Electrolyte solution filling height 5 Cathode red 6 Anode yellow 7 Gas outlet Electrodes A diaphragm is located between the electrodes for generation anode and cathode The diaphragm i...

Page 78: ...rom the measuring gas that could disrupt the analysis The NOx absorber removes nitrogen oxides NOx from the measuring gas High nitro gen oxide content has an influence on the analysis and leads to fal...

Page 79: ...nd HX absorber 1 NOx absorber 2 HX absorber Hose diagram Labeled hoses connect the measuring cell with the other components in the detection module The numbers in the hose diagram correspond to the la...

Page 80: ...detection module on and off is located on the top right of the rear of the device when viewed from the front The device fuse and power connection are located beneath it Communication with the basic mo...

Page 81: ...module and to an earthed socket Observe the permissible maximum voltage Connect the detection module with the basic module via the interface S Coul interface on the rear of the detection module S Cou...

Page 82: ...2 1 2 3 5 6 7 8 4 Figure 53Coulometric sulfur detector with measuring cell without door 1 Indicator electrodes connection 2 Indicator electrode black 3 Gas inlet 4 Measuring cell 5 Port for manual dos...

Page 83: ...he salts have completely dissolved Carefully add 10 ml of glacial acetic acid Keep moving the flask while pouring the acid Carefully shake the solution Fill the volumetric flask with ultrapure water u...

Page 84: ...til the salt has dissolved completed The solution can be kept for approx 1 month in a tightly sealed container Standard solutions can be prepared by diluting the solution 100 l of the diluted solution...

Page 85: ...sis group or create a new one and confirm via OK Create an analysis sequence Enter the sample ID for all sample in the Name field Release all sequence lines Confirm the entries with OK Click the Start...

Page 86: ...R O2 CO2 H2O R Hydrocarbon The radiation sensor is CO2 sensitive The double bond between carbon C and oxy gen O has a specific absorption range in the infrared wavelength band If a ray of light is pro...

Page 87: ...ontal operation mode 11 1 3 Connection The following components can be found on the rear of the device Main switch power connection and device fuses Inlet and outlet for the analysis gas Interface to...

Page 88: ...complete 11 3 Operating the analysis system Switch on the basic module and the detection module The devices boot up The status LED on the front of the basic module light up in green after approx 30 s...

Page 89: ...multi EA 5000 Carbon analysis with the TC module 89 Click the Start Measurement button The prepared analysis sequence is processed For manual sampling follow the instructions in the software...

Page 90: ...ve The double bond between carbon C and oxygen O has a specific absorption range in the infrared wavelength band If a ray of light is projected through a cuvette arrangement the CO2 content in the mea...

Page 91: ...opened 1 Water traps 2 Measuring gas hose from the basic module hose 80 3 Condensate pump 4 TIC reactor 5 Cooling block measuring gas dryer 6 Halogen trap 7 Hose 81 The basic module must be equipped w...

Page 92: ...rked clamp 3 Condensation coil TOC combustion tube The TOC combustion tube reactor is used to determine the TC TOC and NPOC param eters in water samples The combustion tube is made of quartz glass and...

Page 93: ...era tion for this reason The syringes have a gas connection for analyses in NPOC mode The injection volume is 50 to 500 l Optimum measurement results are achieved when 50 to 100 of the volume of the m...

Page 94: ...rom TIC determination is pumped out via the lateral outlet on the glass container The condensate pump transports the waste to the waste outlet on the rear of the device The two following components pr...

Page 95: ...83 84 82 81 80 85 86 Figure 61Hose diagram of the TOC detector Straight and angled FAST connectors are used to fasten hose connections 12 1 3 Connection The device switch for switching the detection m...

Page 96: ...suring gas inlet is connected with hose 82 The purged condensate or waste solution from TIC determination is drained via the waste outlet on the rear of the module For this a waste hose is connected t...

Page 97: ...ule to the basic module via the two interfaces 9 pin interface cable C NDIR interface on the rear of the detection module C NDIR interface on the rear of the basic module 25 pin interface cable extern...

Page 98: ...own in the illustration Insert the TOC combustion tube into the combustion furnace of the basic module Connect the oxygen supply hose 3 Fasten the combustion tube with the tube holder Install the cond...

Page 99: ...tube for EC OC determina tion For EC OC determination the special combustion tube for EC OC determination must be used The measuring gas is routed directly from the combustion tube into the NDIR dete...

Page 100: ...TIC determination Regenerating the TIC reactor 165 Dilute highly acidic and saline samples e g 1 10 Aerosols can form in the TIC reactor during analysis of these samples The capacity of the halogen t...

Page 101: ...t via email for fault diagnosis address on inside of the front cover 13 2 Remedying software message faults Communication problems between the hardware and the software can often be reme died by a bas...

Page 102: ...rrupted No data transfer for 10 s Check port selection 17 Incorrect interface protocol ID Fault after update the program versions of the firmware and multiWin do not match Update required 20 Timeout I...

Page 103: ...ncorrect command structure Communication to the chlorine module inter rupted Acknowledge message Switch the chlorine module on off Initialize 132 Cl sensor Indicator error Indicator value out of range...

Page 104: ...ion interrupted after autosampler de tection during initialization Acknowledge message Initialize 222 Boat Broken Boat defect during removal from the combustion tube only if boat sensor is used Remove...

Page 105: ...Argon missing during dosing No argon applied to LPG module Check gas supply Check gas inlet pressure 253 LPG Incorrect sample volume Dosed volume is not a whole multiple of the sam ple loop inserted A...

Page 106: ...error Acknowledge message Initialize 304 Temperature controller Communication error Temperature cannot be set Acknowledge message Initialize 400 Syringe pump No connection Communication error Acknowl...

Page 107: ...multiWin program in the window The basic initializa tion must always be performed in the following situations Connection of new system components Recognition of system components which were shut down...

Page 108: ...s with sensor values 5 Gas flow displays 6 Furnace temperature horizontal line horizontal installation vertical line vertical installation The displays in the Status analyzer window are color coded Th...

Page 109: ...rack syringe size All sampling modules detected during initialization are displayed and possibly de scribed in detail The following displays are possible Display Description GSS pressureless Gas dosi...

Page 110: ...The following dis plays are possible Display Description C NDIR TC module or TOC module with NDIR detector N CLD CLD 5000 with chemiluminescence detector S UVFD UVFD 5000 and MPO 5000 with UV flouresc...

Page 111: ...tive drift defined in the system Wait for the drift to go back into range this is normal immediately after cell maintenance or af ter commissioning the device Check the maximum drift setting in the me...

Page 112: ...og values outside range Access the values via the System Component test NDIR menu item Running in time Detector not yet ready for operation Wait for the run in period after activation to com plete app...

Page 113: ...onnection and en sure correct fit at the con nection points Pneumatic seal in the coupling not sealing com bustion tube Check Ar supply Flip the toggle switch for the pneumatic seal down Septum incorr...

Page 114: ...n Dosing fault Check dosing by auto in jector or autosampler System leaking Check system tightness Temperature set too low Check temperature con figuration in the method Wrong or unsuitable cali brati...

Page 115: ...ethod with no CLD active Activate a method with nitrogen detec tion Other fault causes Check the condition of the module under System Component test Pressure error Gas outlet flow im peded Check the s...

Page 116: ...lacing the absorber 148 Sample unsuitable for vertical operation mode droplet forma tion Use the horizontal operation mode In vertical operation mode Quartz wool not present or at the wrong position i...

Page 117: ...exces sive nitrogen content Nitrogen compounds cannot be completely converted to NOx due to their structure peptides proteins multiple N N com pounds such as azo dyes polycondensed N compounds such a...

Page 118: ...forma tion Dilute samples if possible Sample unsuitable for vertical operation mode droplet forma tion Use the horizontal operation mode In vertical operation mode Quartz wool not present or at the w...

Page 119: ...only for sulfur detectors with MPO option Absorber on rear of module worn out or incorrectly connected Check connection and replace absorber as necessary Gas hose on the ab sorber leaky or loose Chec...

Page 120: ...S de termination Nitrogen Use MPO technology Dilute samples if possible Incomplete sample incineration pyroly sis products Use a suitable com bustion mode or sampler clean device before continuing wor...

Page 121: ...coulometric sulfur de tector 120 Incorrect electrolyte Create electrolyte see Preparing the measuring cell 83 Filling level in the measuring cell too high or low Fill the measuring cell of to the heig...

Page 122: ...es Homogenize sample before analysis NDIR baseline drift Unfavorable integra tion criteria Integra tion canceled to early Check settings Increase the maxi mum integration time Sample unsuitable for ve...

Page 123: ...gas con nection to the basic module Check the gas quality Check the analog val ues by performing a component test Sys tem menuComponent test NDIR detector faulty Inform customer ser vice department Le...

Page 124: ...cold sam ples Homogenize sample before analysis NDIR baseline drift Unfavorable integra tion criteria Integra tion canceled to early Check settings Increase the maxi mum integration time Sample unsui...

Page 125: ...nge volume Cannula damaged or clogged Replace cannula or re move clogging with a cleaning stylet Filter samples contain ing particles before analysis Inhomogeneous sam ples Inhomogeneous water samples...

Page 126: ...e catalyst System is leaking Check the sluice for leaks Replace septum Incorrect injection vol ume For manual sampling introduce the sample volume set in the method Phosphoric acid in the TIC reactor...

Page 127: ...s necessary Replace combustion tube if it shows cracks devitrification or other damage Replace check valve and inlet filter in the gas box if compo nents are clogged damaged and block the gas flow Che...

Page 128: ...fit Measuring cell high sensitive Check the fill level of the internal electrolyte of the sensor electrode refill as necessary Replace bridge electrolyte if the fill level has dropped to 2 cm below t...

Page 129: ...ck the condensate pump for leaks Check the dosing syringe for leaks Every six months Replace water traps earlier if necessary Annually Replace catalyst in the TOC combustion tube earlier if in structe...

Page 130: ...ve the upper cover of the basic module Open the device door Flip the toggle switch for the pneumatic seal up The auto protection valve assembly is opened Horizontal operation mode with ABD Unscrew the...

Page 131: ...e e g propane For nitrogen and sulfur determination in vertical operation mode Insert a new quartz wool plug in the combustion tube Inserting the quartz wool plug 131 The combustion tube is clean and...

Page 132: ...ne 14 2 4 Installing the combustion tube WARNING Risk of explosion and sooting due to improper connection of the gases to the combustion tube The connections for argon and oxygen on the combustion tub...

Page 133: ...and 4 into the FAST connectors on the combustion tube Re insert the cover plate with hole into the top device opening Connect the autosampler or auto injector 3 4 FS For horizontal operating mode Pres...

Page 134: ...ed However for the installation and removal of the auto protection valve assembly it is not necessary to remove the side panels Exit the multiWin program switch off the basic module via the power swit...

Page 135: ...y from the combustion furnace The installation of the auto protection valve assembly is in reverse order 14 3 2 Check and replace the filter Remove the auto protection valve assembly Check the filter...

Page 136: ...for operation again 14 3 3 Replacing the pneumatic seal Remove the auto protection valve assembly Unscrew the 4 screws attaching the pneumatic seal to the auto protec tion valve assembly Remove the ho...

Page 137: ...lter Place the pneumatic seal onto the auto protection valve assembly and attach it with 4 screws The auto protection valve assembly is ready for operation again 14 4 Replacing the membrane dryer CAUT...

Page 138: ...e into the vertical position Remove hose 5 1 and hose 12 2 Remove hose 13 see arrow Unscrew the 3 knurled screws and remove the holder The membrane dryer is fastened to the furnace with 2 knurled scre...

Page 139: ...ose end must be flush 1 2 3 Figure 66Replacing the Fingertight connections 1 Hose 2 Banjo bolt 3 Conical nipple 14 6 Replacing the septum on the injection port In vertical operation mode the septum on...

Page 140: ...tem have been excluded The check valves are located in the valve block on the gas box on the left side of the device Switch off the basic module and disconnect the power plug from the power outlet Swi...

Page 141: ...o their target values observe the message in the software and possible leaks in the system have been excluded Switch off the basic module and disconnect the power plug from the power outlet Switch off...

Page 142: ...ds is monitored automatically If the system is leaking the Gas leak message will appear in the Status analyzer window and the MFC 1 display is marked in red Starting a measurement is not possible 14 8...

Page 143: ...tronics in the basic module and connect the flow monitoring set hose 2 see arrow Read the current gas flow in the Component test Flow System Compo nent test menu item window The target flow is the sum...

Page 144: ...he control electronics on the right in the basic mod ule System tightness for Cl methods 142 Connect the other end of the hose set with the MFM in inlet on the basic module Read the current gas flow i...

Page 145: ...e basic module via the device switch and disconnect the power plug from the socket Switch off the gas supply Remove the top cover and the doors from the module Remove the left side panel Disconnect th...

Page 146: ...is performed in the reverse order 14 10 Maintenance of the CLD 5000 nitrogen detector 14 10 1Replacing the ozone generator DANGER Risk of electric shock High voltages are present in the interior of th...

Page 147: ...ator Remove the screw the ozone generator is fastened to the base plate with see ar row Carefully push the old ozone generator out of the module and remove it Insert a new ozone generator in the detec...

Page 148: ...e and area with earlier measurements For resuming measuring operations Determine the daily factor to test calibration If the daily factor is outside of the tolerance range the analysis system must be...

Page 149: ...vice which can lead to electric shock if contacted Before opening Switch off the device via the power switch Disconnect the power cable from the socket CAUTION Risk of burns from the thermal ozone dec...

Page 150: ...g hose connections Disconnect hose 25 from the T piece Unscrew hose 24 from the bottom of the ozone decomposers Remove the ozone decomposer with its filter and hose 25 from the holding clamps Recommen...

Page 151: ...the safety data sheet CAUTION Risk of injury A risk of injury due to broken glass is present when handling glass parts Handle glass parts with extreme caution The sulfuric acid absorbs the water that...

Page 152: ...the heated gas transfer line from the sulfuric acid con tainer Remove the thin hose from the container CAUTION Sulfuric acid residue can still be present on the hose Empty all of the sulfuric acid in...

Page 153: ...operation for multiple days clean the measur ing cell and store it in a dry place Check the casing of the magnetic stirring rod for cracks regularly If metal ions from the stirring rod come into conta...

Page 154: ...with ethanol Insert the combined electrode in the measuring cell and allow the solution to stir for several hours in the detection module Do not connect the measuring cell or the electrode to their el...

Page 155: ...he end of a working day or the end of a working week the electrode requires a stabilization period of 2 to 24 hours depending on its degree of aging Fill the sensor electrode up to shortly below the f...

Page 156: ...can show discoloration from longer use 14 12 Maintenance of the UVFD 5000 and MPO 5000 sulfur detector 14 12 1Replacing the UV lamp WARNING Risk of electric shock High voltages are present in the inte...

Page 157: ...limit can no longer be reached Check the state of the UV lamp in the System Component test menu in the detec tion module tab If a defect is indicated or the lamp is worn out replace the lamp Switch of...

Page 158: ...in 14 12 2Replacing the chemical ozone decomposer Only for the MPO 5000 Replace the entire chemical ozone decomposer at least once annually Always replace the ozone decomposer when the smell of ozone...

Page 159: ...rber once per week Replace the filling if necessary Replace the filling of the NOx absorber if the color has turned from light green to yellow or light brown Replace the filling of the HX absorber if...

Page 160: ...Maintenance and care multi EA 5000 160 1 2 Figure 74NOx absorber and HX absorber 1 NOx absorber 2 HX absorber...

Page 161: ...hen it is used up Switch of the magnetic stirrer via the rotary switch Switch off the detection module via the power switch Disconnect the two electrode cables on the generation and indication connect...

Page 162: ...he magnetic stirrer set to stage 3 approx NOTICE The magnetic stirring rod can damage the electrodes if the rotation fre quency is set too high Operate the rotary switch with care Wait for approx 5 mi...

Page 163: ...small water trap must face upward Insert the new water traps into the clamps The large water trap has to be positioned at the bottom Connect the hose connections to the water traps NOTICE For angled F...

Page 164: ...Clamp Replace the contents of the halogen trap when half of the copper wool is discolored Remove the FAST connectors from the halogen trap and remove the U tube from the clamps Remove the quartz wool...

Page 165: ...determination or TIC determination in differential mode The TIC reactor must be regenerated daily How often this must be done is dependent on the TIC content of the samples For high TIC content regene...

Page 166: ...r Remove the waste hose hose 86 to the condensate pump from the connection on the bottom of the TIC reactor Remove the TIC reactor from the detection module and check it for deposits and cracks Rinse...

Page 167: ...om the pump s connections Remove the guide piece with the pump hose from the pump body Check the pump hose and the connections on excessive wear and cracks Wipe the pump body and roller carrier with u...

Page 168: ...t of the TOC combustion tube with the condensation coil Remove the fork clamp and disconnect the spherical joint connector Remove the FAST connector on the bottom end of the condensation coil Carefull...

Page 169: ...via the power switch and allow the device to cool Switch off the gas supply and disconnect the power plug from the power outlet Open the doors of the basic module and remove the top cover Remove the...

Page 170: ...Cover the ground quartz glass with a piece of high temperature fiber mat HT mat layer height approx 1 cm Close the filled TOC combustion tube with septum and screw cap and reinstall it in the furnace...

Page 171: ...owing when moving the device within the laboratory Insufficiently secured components pose a risk of injury Before moving the device remove all loose parts and disconnect all connections from the devic...

Page 172: ...tube Maintenance of the multi purpose combustion tube 129 Remove the auto protection valve assembly Maintenance of the auto protection valve assembly 134 Remove the membrane dryer with holder from th...

Page 173: ...ply Disconnect all connections on the rear of the detection module Seal the open gas connections with the ends of a short fitting piece of hose to pre vent contamination during transport Remove loose...

Page 174: ...connections Disconnect the hose connections to the HX and NOx absorbers and remove both ab sorbers from the module Remove the measuring cell from the module Remove the electrodes and the gas inlet tub...

Page 175: ...electrodes in accordance with applicable regulations on hazardous waste The chemical ozone decom poser on the absorber of the CLD 5000 or MPO 5000 The chemical ozone decomposer contains metal oxides T...

Page 176: ...e into the multi purpose combustion tube via injection port with septum EOX Direct injection of an extract into the multi purpose com bustion tube via injection port with septum TC NPOC Direct injecti...

Page 177: ...olume TS TN TX TC TOC Liquids 1 to 100 l horizontally with ABD 1 to 500 l vertically with MMS or TOC module and direct manual dosing Solids 0 001 to 110 mg Non pressurized gases 1 to 100 ml Pressurize...

Page 178: ...trolled via software settings for the ABD Measuring gas dryer TS TN TC EC OC Membrane dryer TX AOX EOX Concentrated sulfuric acid TOC NPOC TIC Condensation through Peltier cooling Detection modules T...

Page 179: ...ml min Membrane dryer drying flow Approx 500 ml min Argon Purity 4 6 Inlet pressure 600 kPa 6 bar Consumption Combustion 100 to 200 ml min Post combustion 0 ml min Pneumatic seal switch Argon must be...

Page 180: ...uency 50 60 Hz Module fuse protection Number of device fuses T 4 0 A H 2 Typical average power consumption 200 VA Interface to the basic module RS 232 Only use original fuses from Analytik Jena Gas su...

Page 181: ...0 to 1000 g Generator current 10 mA Electrolyte volume 120 ml Electrical variables Power supply 110 to 240 V 10 5 Overvoltage category II Frequency 50 60 Hz Module fuse protection Number of device fus...

Page 182: ...lometric titration Measuring range S in sample 0 to 40000 mg l S Measuring range S absolute 0 to 200 g S Electrical variables Power supply 110 to 240 V 10 5 Overvoltage category II Frequency 50 60 Hz...

Page 183: ...bon TC TIC TOC NPOC EC OC Sample feed for TIC analysis Direct injection in the TIC reactor Detection principle NDIR non dispersive infrared absorption spectrometry Measuring range C in aqueous samples...

Page 184: ...e directive 2011 65 EU The device is designed and tested in accordance with standards meeting the require ments of EU directives 2014 35 EU and 2014 30 EU The device leaves the factory in a sound cond...

Page 185: ...brane dryer 29 Figure 18 Space required for the basic device and modules vertical operation 33 Figure 19 Space required for the basic device and modules horizontal operation 34 Figure 20 Media connect...

Page 186: ...c module 92 Figure 58 TOC combustion tube unfilled 92 Figure 59 Tube holder for the TOC combustion tube 93 Figure 60 Condensation coil 94 Figure 61 Hose diagram of the TOC detector 95 Figure 62 Rear o...

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