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Function and design

multi N/C pharma HT

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Figure 10Combustion furnace

3.1.4

Measuring gas drying and cleaning

Condensation coil

The glass condensation coil is located to the right of the furnace and is attached to the
outlet of the combustion tube.

The condensation coil quickly cools the measuring gas. The water vapor contained in the
measuring gas condenses. The measuring gas and water mixture is routed to the TIC
condensate container via a hose.

Figure 11Condensation coil

1 Hose 1 to the TIC condensate container

2 Condensation coil

TIC condensation module

The TIC condensation module consists of a TIC condensate container and a cooling
block. The TIC reactor and the gas/liquid separator are combined in the TIC condensate
container. The cooling block dries the measuring gas at the same time.

The TIC condensation module is located on the left front side. The measuring gas/water
mixture is supplied via the top left connection via hose 1.

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Содержание analytikjena multi N/C pharma HT

Страница 1: ...Operating Manual multi N C pharma HT TOC TNb Analyzer...

Страница 2: ...trasse 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 0112 001 23 Edition C 12 20...

Страница 3: ...ls 12 2 4 6 Safety instructions maintenance and repair 13 2 5 Behavior during emergencies 14 3 Function and design 15 3 1 Layout 15 3 1 1 Sample supply system 16 3 1 2 Hose system 17 3 1 3 Combustion...

Страница 4: ...ion results 70 5 4 3 Editing calibration 71 5 4 4 Linking a calibration to a method 71 5 4 5 Managing calibration data 73 5 5 Performing measurements 73 5 5 1 Measurement with manual sample feed 73 5...

Страница 5: ...iluminescence detector CLD 104 7 Troubleshooting 105 7 1 Software error messages 105 7 2 Status errors 110 7 3 Device errors 112 8 Transport and storage 115 8 1 Transport 115 8 1 1 Preparing the analy...

Страница 6: ...Table of contents multi N C pharma HT 6...

Страница 7: ...d 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 program are indicated as follows Program ter...

Страница 8: ...d the device The analyzer may only be used to determine the total carbon content and the concen tration of organic and inorganic bound carbon in aqueous samples The analyzer is particularly suited for...

Страница 9: ...ave been attached to the de vice Warning symbol Meaning Comment Warning against hot surface On the furnace on the furnace cover On the left side wall Risk of burns from the hot furnace Warning against...

Страница 10: ...ns transport and commissioning Incorrect installation can create serious hazards This may result in electric shock and explosion if the gases are not connected correctly Only the Analytik Jena GmbH cu...

Страница 11: ...ad to limitations regarding the warranty and access to customer service Keep all combustible materials away from the device The furnace operates at temperatures of 700 to 950 C Do not touch the hot co...

Страница 12: ...ar of the housing if there is any malfunction of the electrical components Disconnect the power plug from the power socket 2 4 4 Safety instructions for the operation of compressed gas containers and...

Страница 13: ...ng is wipe disinfection If the dis infectant has a spray nozzle apply disinfectant to a suitable cloth before using it on the device Particular care must be taken if infectious materials are analyzed...

Страница 14: ...s If there is no immediate risk of injury switch off the device and the connected system components immediately in hazardous situations or in the event of an accident and or disconnect the power plugs...

Страница 15: ...d by the user can be accessed via the two doors on the front the left hand removable side wall or the top cover The analyzer consists of the following main components Sample supply system Gas box and...

Страница 16: ...ringe pump with 2 port valve The in jection volume is 50 to 3000 l The hose connections are attached to the 2 port valve using Fingertight screw connec tions The syringe body is made of glass and repl...

Страница 17: ...NDIR Halogen trap Water traps Drying V3 Figure 4 Hose diagram Components for flow adjust ment The analyzer automatically sets the carrier gas flow and controls the inlet flow via an MFC Mass Flow Cont...

Страница 18: ...C determina tion out automatically after each measurement The condensate pump is located behind the front doors next to the halogen trap Figure 6 Condensate pump Phosphoric acid pump The phosphoric ac...

Страница 19: ...olt finger tight 1 2 3 Figure 9 Fingertight screw connection 1 Hose 2 Banjo bolt 3 Conical nipple 3 1 3 Combustion system The combustion system is behind the left side wall of the analyzer The combust...

Страница 20: ...ng gas and water mixture is routed to the TIC condensate container via a hose Figure 11Condensation coil 1 Hose 1 to the TIC condensate container 2 Condensation coil TIC condensation module The TIC co...

Страница 21: ...after each measurement Figure 12TIC condensation module 1 TIC condensate container 2 Connection for hose 1 condensation coil measuring gas feed 3 Cooling block 4 Connection to the water traps 5 Water...

Страница 22: ...rotects the detectors and the flowmeter in this manner The halogen trap is installed in the gas path behind the TIC condensate con tainer and the water traps The halogen trap consists of a U shaped tu...

Страница 23: ...n for TOC analyses The measuring gas flow is determined in parallel with the NDIR signal in the VITA method The NDIR signal is normalized via computer control This compensates for oc curring flow fluc...

Страница 24: ...analyzer Figure 16LED strip right door open 1 Broken thermocouple is lit when a thermocouple is defective 2 Furnace comperator is lit at excessive temperatures 3 Furnace heating on off 4 Device volta...

Страница 25: ...ear The type plate contains the following infor mation Manufacturer with complete address Trade name and model indication Serial number Electrical connection data CE mark and WEEE disposal mark 3 1 7...

Страница 26: ...es temperatures of up to 950 C are achieved The digestion is supported by catalysts 3 3 Function and measuring principle The analyzer is a compact high performance device for determination of the cont...

Страница 27: ...r nitrogen in the measurement solution Afterwards the calcula tion of the carbon or nitrogen content in the sample is performed via a previously deter mined calibration function 3 4 Measuring methods...

Страница 28: ...rged organic substances NPOC analysis according to the NPOC plus method This method was developed especially for the detection of low TOC content in samples with high TIC content or a high level of di...

Страница 29: ...g the furnace temperature to temperatures below the melting point of the salts is recommended with high salt matrices e g seawater Alternatively a CeO2 catalyst can be used at a reaction temperature o...

Страница 30: ...in the multiWin soft ware Not all parameters require calibration however You can store up to three calibration functions for different concentration ranges for each parameter in a method The software...

Страница 31: ...and TIC channels NPOC plus The calibration of the NPOC plus method is the same as the calibration of the TOC Diff method Before analysis the TIC must be sufficiently purged for the use of the differe...

Страница 32: ...en probability 3 6 5 Other calculations For all measurements where multiple injections are carried out the average value AV the standard deviation SD and the variation coefficient VC are calculated an...

Страница 33: ...ely or entered manually in the software The software takes the dilu ent blank value into account when calculating the concentration of diluted samples The diluent blank value can change over time and...

Страница 34: ...to account If samples are measured with the so called eluate method the software automatically subtracts the integral of the blank value from the integral of the sample measurement Ieff IRaw IEluate b...

Страница 35: ...quinone and TOC water that also has a concentration of 500 g l to check system suitability This corresponds to a concentration of 0 75 mg l p benzoquinone Determine the TOC concentrations of the refer...

Страница 36: ...ture 5 to 55 C Humidity during storage 10 to 30 use desiccant Operating altitude max 2000 m 4 1 2 Device layout and space requirements The basic device has been designed as a compact bench top device...

Страница 37: ...ation of the electrical equipment in the laboratory must comply with the DIN VDE 0100 standard At the connection point an electrical current in accordance with the standard IEC 60038 must be available...

Страница 38: ...transport packaging Retain the transport packaging for future transport Place the analyzer at its intended location Remove the adhesive tape from the doors and side walls Remove the adhesive tape fro...

Страница 39: ...connection 4 CLD gas connection 5 O2 Air carrier gas connection 6 Connection of the neutral conductor on the autosampler 7 waste connection 8 RS 232 interface for sampler autosam pler 9 RS 232 interf...

Страница 40: ...carrier gas hose to the O2 Air gas connection on the rear of the device To do this insert the hose in the quick release connector To release the hose again later press the red ring back and pull the h...

Страница 41: ...be equipped with two canulas This allows the autosampler to au tomatically purge samples for NPOC analysis During NPOC analysis the sample is acidified outside the analyzer with diluted acid to a pH v...

Страница 42: ...with screw con nection 7 Purging canula with screw connection The autosampler can be equipped with two canulas This allows the autosampler to au tomatically purge samples for NPOC analysis The autosam...

Страница 43: ...ttached to the right hand side of the analyzer by means of the supplied holder Alternatively the autosamplers can be placed next to the analyzer Figure 24Autosampler attached to the analyzer by means...

Страница 44: ...off Switch off the analyzer before installing the autosampler Plug the grounding conductor into the connection on the rear of the analyzer Con nect the grounding conductor to the connection on the bo...

Страница 45: ...21hp autosamplers only Place a magnetic stirring rod in the sample vessel Insert the canulas in the canula holder To do this guide the two canulas through the sleeve with two holes for sequential purg...

Страница 46: ...etup tool Select the autosampler type in the Sampler list Exit the multiWin set up tool window with Create Start the multiWin program and initialize the analysis system Open the Options window with me...

Страница 47: ...om the magnetic stirring rod so that the rod can move freely and does not damage the canulas When adjustment is complete exit the window with Save The autosampler is ready for operation 4 3 1 2 Conver...

Страница 48: ...stalling and commissioning the sampler 44 4 3 2 AS vario autosampler CAUTION Risk of injury from moving parts There is a risk of injury in the movement range of the sampler arm For example hands or fi...

Страница 49: ...to the analyzer It can be equipped with 2 canulas Figure 30Layout of the AS vario autosampler 1 Connection hose to the analyzer purg ing hose for NPOC measurement 2 Connection hose to the analyzer sa...

Страница 50: ...ayout of the AS vario ER autosampler 1 Canula for connection to the sample in take hose 2 Canula holder here with no 72 3 Sample tray for 72 4 Ultrapure water bottle 5 Canula flush 6 Canula for connec...

Страница 51: ...e liquid Place the sample tray on the autosampler Ensure that it clicks into place Check that the correct canula holder is installed on the autosampler arm The num ber engraved on the bottom must matc...

Страница 52: ...with Start Program files multi Win multiWin setup tool Select the autosampler type in the Sampler list Exit the multiWin set up tool window with Create Start the multiWin program and initialize the an...

Страница 53: ...e hose in connection 2 Place the hose end in the waste container NOTICE Route the outlet tube at a constant downward incline If necessary shorten the hose The hose must not dip into the liquid Adjust...

Страница 54: ...ng operation Only carry out manual adjustment when the device is switched off The autosampler has a piercing function for sample vessels with septum caps The sam pler can be equipped with 1 to 2 canul...

Страница 55: ...s Figure 39Electrical connections 1 Power supply unit connection 2 Device switch 3 Connection to the analyzer 4 Not used 5 Stirrer connection Commissioning the autosam pler Remove the transport lock R...

Страница 56: ...r so that enough space is provided behind the device for the motion range of the autosampler arm as well Connect the low voltage side cable of the table power supply unit to the rear of the autosample...

Страница 57: ...vessels basic position Figure 42Canula position for NPOC measurement with parallel left and non paral lel right purging Secure the canulas by slightly tightening the knurled head screws Connect the h...

Страница 58: ...hange the configuration Exit the multiWin program Start the setup tool in the Windows interface with Start Program files multi Win multiWin setup tool Select the autosampler type in the Sampler list E...

Страница 59: ...zer gas connection 10 out sample outlet gas 11 Adsorber cartridge removes NOx from the waste air Technical data Detection principle Chemiluminescence detector Parameter TNb total bound nitrogen Measur...

Страница 60: ...tch on the detector The status LED indicates operational readiness Checking and changing the configuration Switch on the analyzer and the detector Start the multiWin program and initialize the analysi...

Страница 61: ...eighed into boats and pushed into the combustion tube with the aid of the manual sample feed The furnace lock can be opened and closed manually via the interlock Combustion system The integrated solid...

Страница 62: ...ned combustion tube with your hands during filling Wear protective gloves Only fill completely dried combustion tubes Wipe off any finger marks with a cloth wetted with pure alcohol Assemble the modul...

Страница 63: ...as follows Remove the combustion tube for vertical operation Remove the sealing plug from the horizontal opening of the combustion furnace Place the plug on the vertical opening of the furnace see im...

Страница 64: ...e end to the module with the Fingertight connection Connect the plug in connector of the analyzer to the left side of the mod ule The software detects that an integrated solids module is connected to...

Страница 65: ...ove the hose of the water trap on the front side To acidify samples use analytically pure acid HCl 2 mol l and make it out of con centrated acid and TOC water For TIC detection only use orthophosphori...

Страница 66: ...nd in good working order All optional accessories autosamplers solids modules etc are connected Prepare the sample and switch on the analyzer as follows Open the valve on the pressure reducer of the g...

Страница 67: ...ed with ultrapure water The gas flow is switched off and the standby temperature is set Switching off the device before extended standstill periods Recommendation Switch off the analyzer before extend...

Страница 68: ...isting cali bration table Carry out the software instructions that follow The Calibration Data of new calibration window opens Figure 46Data for new calibration Select the calibration type in the Cali...

Страница 69: ...ered in the input field Complete the calibration table for each parameter in accordance with the standard solutions provided In the Rep column the software automatically accepts the number of repeat m...

Страница 70: ...ation results tab compiles the results for each calibrated parameter Figure 48Performed calibration data Calibration results tab Results table Display of Number of detections Target concentration used...

Страница 71: ...olumn Enabling disabling measured values for preparation water You can view the individual measured value determined for the preparation water by clicking on the Edit button You can then activate or d...

Страница 72: ...icients are displayed in the left and right columns One or two calibration ranges exist Expanding existing calibration ranges Accept the new calibration data with the Accept values button The software...

Страница 73: ...default multiWin CSV The directory is selected in the Options window in the Files and Directories tab Open the window with the Configuration Edit options menu option Export to clipboard Reopening a ca...

Страница 74: ...ngs tab The new fields are displayed in the Measurement start window in the FreeStrings tab You can fill the fields with sample information See also 2 Troubleshooting 105 5 5 2 Measurement with autosa...

Страница 75: ...le data window with Start Open an existing rack table and add to it Or Enter the sample ID in the Sample ID column in the new rack table Check the sample tray assignment for this If necessary enter th...

Страница 76: ...sample feed are possible with the integrated solids module When creating a method for solids analysis select the Horizontal Furnace option Click on Start measurement Enter the sample ID and the sample...

Страница 77: ...drip tray Check the fastening screws for tight fit Sample supply system and autosampler Maintenance interval Maintenance task Quarterly Check the syringe pump for leaks Every 12 months Clean the dosin...

Страница 78: ...furnace lock for leaks Every 12 months Clean the combustion tube earlier if required When necessary After software notification at the latest Check the catalyst Replace as necessary Replace a worn sea...

Страница 79: ...with the Instrument Sampler Alignment menu option Select needle in the list field in the Please select position needing adjustment group The autosampler arm moves over the adjustment points on the sam...

Страница 80: ...timized Click on Save to save the adjustment values Open the Sampler Alignment window again Move to the flushing position and posi tion 1 with the buttons to check The autosampler is adjusted Adjustin...

Страница 81: ...tip does not immerse in the sample vessel Open the window of the same name with the Instrument Sampler Alignment menu option Adjust the immersion depth of the sample intake canula into the wash cup a...

Страница 82: ...herwise possible in the sample vessel Adjust the flushing position Adjust the x and y axis positions so that the canula is located in the middle of the wash cup Adjust the special canula in the z axis...

Страница 83: ...tion fur nace Set the NPOC purge flow as follows Figure 56Grounding conductor connection on the side wall Open the left side wall of the analyzer Push the accessory modules to the side if nec essary D...

Страница 84: ...e needle valve to the left Decrease the NPOC purge flow Turn the needle valve to the right Check the flow indication in the System state window when doing this The current NPOC purge flow is displayed...

Страница 85: ...od of the new dosing syringe into the drive Screw the glass cylinder onto the valve The analyzer is ready for operation again 6 4 Replacing the pump hose CAUTION Risk of chemical burns during hose rep...

Страница 86: ...intact or new pump hose back into the guide piece Align the hose clamps downward during installation Insert the hose guide in the groove of the guide piece Position the guide piece around the pump bod...

Страница 87: ...glass components Use the threading aid to feed thin hoses into the connectors This is included with the analyzer Check the system for leaks after hose replacement Slide the FAST connector onto the ca...

Страница 88: ...only tighten it hand tight 1 2 3 Figure 60Replacing the Fingertight connection 1 Hose 2 Banjo bolt 3 Conical nipple 6 6 Checking the system for leaks NOTICE Risk of gas leakage When the outlet flow i...

Страница 89: ...p benzoquinone Dispose of the catalyst in accordance with disposal regulations See also 2 Disposal 119 6 7 1 Removing the combustion tube CAUTION Risk of burns at the hot furnace Switch off the devic...

Страница 90: ...the combustion tube Remove the union nut the pressure ring and the three sealing rings Remove the used catalyst filling Check the combustion tube for heavy crystallization cracks and burst spots Only...

Страница 91: ...ass wool 1 into the combustion tube approx 1 cm high carefully press it down with a glass rod and press it into place The glass wool holds back the catalyst Ensure that no catalyst can get into the ga...

Страница 92: ...mat into the combustion tube and push it down with a glass rod until the catalyst is covered Only press the mat down lightly onto the catalyst The recommended operating temperature for this filling i...

Страница 93: ...the union nut hand tight The furnace canula and the carrier gas canula have already been attached to the furnace head If it is not present insert the ceramic holder into the top opening of the combus...

Страница 94: ...ply Connect the power plug with the socket and switch on the analyzer via the main switch Check the system for leaks The analyzer is ready for operation again 6 8 Removing and installing the combustio...

Страница 95: ...rom interfering with installation Unscrew the knurled head screws on the device bottom the furnace is fastened with Insert the furnace in the middle Align the front side of the furnace to be parallel...

Страница 96: ...1 AD and BB with FAST connectors off of the TIC condensate container Disconnect waste hose 11 from the bottom connection on the TIC con densate container Unscrew the 2 knurled head screws on the cover...

Страница 97: ...ews The screws are captive and re main attached to the wall Remove the protective grounding Set the side wall aside safely Pull hose 1 out of the FAST connector of the condensation coil Release the jo...

Страница 98: ...ll Slightly tighten the screws first on the bottom side and then on the top side Tighten the screws in turns Open the gas supply Connect the power plug with the socket and switch on the analyzer via t...

Страница 99: ...rosol trap must face downward The labeling on the small water trap disposable retention filter must face up ward Connect the large water trap with the lower hose Press the water traps into the clamp s...

Страница 100: ...sconnect the power plug from the socket Allow the analyzer to cool down Open the left side wall of the analyzer Push the accessory modules to the side if nec essary Do not kink any connection hoses Un...

Страница 101: ...the power plug with the socket and switch on the analyzer again via the main switch Check the system for leaks The water traps on the front side and the gas box are replaced See also 2 Checking the s...

Страница 102: ...rinse the U tube with ultrapure water and allow it to dry well Fill the U tube with new copper wool and brass wool using tweezers or a small hook Replace the complete contents of the U tube Do not pac...

Страница 103: ...the carrier gas outlet of the gas box Remove the angled FAST connector from the gas box connection Attach the straight FAST connector Unscrew the other hose end from the solids module Remove the fork...

Страница 104: ...ich exits the detector at the out outlet The cartridge is filled with active carbon and soda lime Do not open the cartridge Dis pose of the used cartridge as a whole in accordance with the local regul...

Страница 105: ...0 ml min from the target flow For fault analysis log files can be recorded After consulting customer service activate log file recording The software stores the log file in the multiWin LOG directory...

Страница 106: ...e Error message 5 Communication error analyzer STAT MESS STEP or INIT Cause Remedy Communication error Initialize the analyzer Error code Error message 4 Communication error analyzer Cause Remedy Comm...

Страница 107: ...e During analysis of highly saline samples salt deposits can form in the combustion tube HT mat used up by analysis of highly saline samples Replace the HT mat in the combustion tube or replace the ca...

Страница 108: ...ssage 112 Swivel drive error Cause Remedy The drive is incorrectly positioned e g jammed The drive is faulty Initialize the analyzer If the error cannot be corrected contact the service Error code Err...

Страница 109: ...ized Cause Remedy The analyzer is not yet initialized after switching on Reset of the syringe pump Initialize the analyzer Error code Error message 409 Syringe pump pump sluggish Cause Remedy A hose l...

Страница 110: ...ontainer is leaky The connections on the water trap sys tems are loose after water trap replace ment or halogen trap maintenance Check the screw connections for com pleteness and deformations Tighten...

Страница 111: ...e on the TIC condensate container The formation of condensation water on the cooling block indicates that the cooling is working The MFC is faulty Inform the service Error indication In Out 0 ml min C...

Страница 112: ...vent the addition of CO2 or organic vapors from the ambient air Check the ambient conditions and rem edy the source of the fault Cover the sample vessels on the au tosampler with aluminum foil Treat t...

Страница 113: ...Measure one or two sample vessels with acidified ultrapure water per analysis series Replace the catalyst After replacing the catalyst perform cal ibration Error Low results for TIC analyses TC TOC N...

Страница 114: ...ply or electronics fault Check the electrical connections Check the laboratory power supply Device fuse faulty Inform the service Error Status LED on the analyzer not lighting Lockin Cause Remedy The...

Страница 115: ...jury A risk of injury due to broken glass is present when handling glass parts Handle glass parts with extreme caution NOTICE Risk of device damage due to unsuitable packaging material Only transport...

Страница 116: ...screws are captive and remain attached to the wall Remove the protective grounding Set the side wall aside safely Carefully remove the condensation coil from the holder empty it and set it aside safel...

Страница 117: ...ockwise up to the stop The drives are in the correct position Slide the transport lock into the opening of the bottom plate up to the stop Fasten the transport lock with the screw and the supplied hex...

Страница 118: ...the legally mandated limits for lifting and carrying loads without auxiliary means Observe the installation conditions at the new location 8 2 Storage NOTICE Risk of device damage due to environmental...

Страница 119: ...ll receive the information regarding recy cling or disposal Catalyst The special catalysts contain Pt Al2O3 or CeO2 Dispose of the used catalyst properly in accordance with the legal disposal requirem...

Страница 120: ...rement range with the HT 1300 solids module 0 to 500 mg Nitrogen detection Nitrogen detection principle optional CLD TNb measurement range 0 to 20000 mg l Process control Control and analysis software...

Страница 121: ...esolution Min 3 2 GHz Min 40 GB Min 4 GB Min 1280 x 780 USB port Min 1 USB 2 0 interface for connecting the basic device CD DVD drive For software installation Operating system Windows 10 or higher Wi...

Страница 122: ...ndition with regard to technical safety To maintain this condition and to en sure safe operation the user must strictly observe the safety and operating instructions contained in this operating manual...

Страница 123: ...A 2021 01 1st version note New version labeling after introduction of the Document Management System A B etc Change of the company s legal form B 2021 11 Inclusion in content management system C 2021...

Страница 124: ...ure 20 Device rear 39 Figure 21 AS 10e autosampler 41 Figure 22 AS 21hp autosampler 42 Figure 23 Parallel purging left and sequential purging right 43 Figure 24 Autosampler attached to the analyzer by...

Страница 125: ...76 Figure 51 Adjusting the autosampler 79 Figure 52 Adjustment points on the sample tray 79 Figure 53 Installing canulas 2 canulas for parallel purging here 81 Figure 54 Adjusting the autosampler 81 F...

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