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multi N/C 2100S (duo, pharma)

Installation and commissioning

4.3.2

Chemiluminescence detector (CLD)

Figure 23Chemiluminescence detector (CLD)

1 Status LED

2 Mains switch

3 Fuse holder

4 Power connection

5 RS 232 connection to the analyzer

6 Service connection

7 Programming switch (service only)

8 Carrier gas connection (O

, synthetic/

purified air)

9 "sample in" analyzer gas connection

10 "out" sample outlet (gas)

11 Adsorber cartridge (removes NO

from

the waste air)

Technical data

Detection principle

Chemiluminescence detector

Parameter

(total bound nitrogen)

Measurement range

0 to 200 mg/l TN

Detection limit

0,05 mg/l TN

Analysis time

3 to 5 min

Gas for ozone generation

Gas supply as for basic device

60 ml/min, 400 to 600 kPa

Dimensions (W x H x D), weight

300 x 470 x 550 mm , 12.5 kg

Electrical connection

110 to 240 V, 50/60 Hz

Fuses

2 T4.0 A H

Typical average power consumption

200 VA

Analyzer interface

RS 232

Содержание Analytik Jena multi N/C 2100S

Страница 1: ...Operating Manual multi N C 2100S duo pharma TOC TNb Analyzers...

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 0109 001 23 Edition C 12 20...

Страница 3: ...terials 13 2 4 6 Safety instructions maintenance and repair 14 2 5 Behavior during emergencies 15 3 Function and design 16 3 1 Layout 16 3 1 1 Sample supply system 17 3 1 2 Hose system 18 3 1 3 Combus...

Страница 4: ...a method 58 5 4 5 Managing calibration data 60 5 5 Performing measurements 60 5 5 1 Measurement with manual sample feed 60 5 5 2 Measurement with autosampler 62 5 6 Operating the integrated solids mod...

Страница 5: ...error messages 93 7 2 Status errors 97 7 3 Device errors 99 8 Disposal 104 9 Transport and storage 105 9 1 Transport 105 9 1 1 Preparing the analyzer for transport 105 9 1 2 Moving the device in the...

Страница 6: ...Table of contents multi N C 2100S duo pharma 6...

Страница 7: ...y particular attention to the information on switching between liquid and solid operation given there The multi N C 2100S pharma model is a special model for pharmaceutical nitrogen analysis Please ob...

Страница 8: ...n be analyzed thanks to special analysis modes NPOC plus Use in power plants and laboratories With its dynamic measurement range the analyzer provides TOC detection for power plants and in industrial...

Страница 9: ...al carbon content in solids can be determined No flammable liquids or substances that can form explosive mixtures may be analyzed with the analyzer Do not analyze concentrated acids with the analyzer...

Страница 10: ...ls have 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 aga...

Страница 11: ...tions 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...

Страница 12: ...y lead 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 ho...

Страница 13: ...e rear 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...

Страница 14: ...ousing 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 analy...

Страница 15: ...ncies 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 p...

Страница 16: ...onents of the analyzer operated or serviced 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 co...

Страница 17: ...tolerance The septum lock is included in the pharma model but it is not used Septum free lock A septum free lock is used as a TC lock The TC lock is used for sample supply for TC and TN analyses The l...

Страница 18: ...croliter syringes with special geometry and a gas connection for NPOC analy ses are used for the autosamplers The syringes have no graduation and are therefore not suitable for manual operation 3 1 2...

Страница 19: ...tion gases The NPOC purge flow can be set via the needle valve on the gas box The needle valve can only be accessed when the left side wall has been removed The NPOC purge flow is measured with an MFM...

Страница 20: ...vide a tight transition between the hoses and connections with different diameters The soft sleeves prevent the risk of glass breakage in comparison to rigid screw connections There are different conn...

Страница 21: ...on coil and TIC condensation module The condensation coil and TIC condensation module are mounted on a carrier plate that is attached on the right hand side of the combustion furnace The glass condens...

Страница 22: ...s not determined here Figure 12Condensation coil and TIC condensation module 1 Condensation coil 2 Cooling block 3 TIC condensate container Water traps The water traps remove interfering components fr...

Страница 23: ...o protects 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...

Страница 24: ...the electrochemical NO detector can be used The NO detector is be hind the right side wall of the analyzer It analyzes the nitrogen oxide NO content in the measuring gas After thermal oxidation of the...

Страница 25: ...erational readiness Figure 15Status LED The LED strip behind the right door indicates different operating states of the analyzer Figure 16LED strip right door open 1 Broken thermocouple is lit when a...

Страница 26: ...ction 8 NPOC NPOC purge gas connection 9 O2 Air carrier gas connection 10 aux gas auxiliary gas connection for pneumatically operated locks 11 waste connection 12 RS 232 interface for sampler autosam...

Страница 27: ...e standard sample tray has 60 positions for 8 ml vessels At low sample volumes a tray with 112 positions for 1 8 ml HPLC snap cap vials can be used Automatic acidifica tion is not possible in NPOC ope...

Страница 28: ...carbon and nitrogen compounds to be converted quantitatively The sample aliquot is dosed directly into the hot zone of the filled reactor combustion tube Here the pyrolysis and oxidation of the sampl...

Страница 29: ...alysis the total organic bound carbon contained in the sample is detected TOC determination is carried out in the analyzer using the differential method which can be described with the following formu...

Страница 30: ...medi ately before the analysis of the sample the greater part of the carbon dioxide generated is purged externally Afterwards the remaining organic carbon TOC from the sample prepared in this manner i...

Страница 31: ...he expected sample concentrations Multiple standard solu tions are measured with the selected method Multiple point calibration with constant concentration Additionally a multiple point calibration wi...

Страница 32: ...k0 k1 k2 calibration coefficient The net integral is the raw integral corrected by the blank value of the preparation wa ter You can specify the regression type linear or quadratic Individual measurin...

Страница 33: ...cTN f ITN The calculated parameters appear in the method in the TN analysis channel 3 6 4 Method characteristics Remaining standard deviation The remaining standard deviation remaining variance expre...

Страница 34: ...t least one combination is smaller than the specified maximum value no further measurements are carried out The software determines the analysis result from the combination of measured values with the...

Страница 35: ...ns of the primary probe in total proportions e g 10 parts in 100 parts This means that 10 ml of the primary sample is filled to a total volume of 100 ml with dilution water A 1 1 dilution ratio equals...

Страница 36: ...of the sample measurement Ieff IRaw IEluate blank value Ieff Effective integral IRaw Raw integral IEluate blank value Eluate blank value 3 7 3 Boat blank value For solids methods the user can determi...

Страница 37: ...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 The required space depends on all the...

Страница 38: ...device to a properly grounded socket which complies with the volt age indicated on the device s rating plate Do not use an adapter in the feeder The device operates on single phase alternating current...

Страница 39: ...ou may want to transport the device again or store it You can recommission the analyzer as described below Analytik Jena always recommends installation via customer service Carefully remove the basic...

Страница 40: ...eutral conductor on the autosampler 2 Power switch main switch 3 FUSE mains fuse holder 4 Main plug mains connection 5 analyte gas connection connected to internal connection via hose bridge 6 CLD pum...

Страница 41: ...cting the gases You are responsible for the gas supply in the laboratory Ensure that the inlet pressure on the pressure reducer is set between 400 to 600 kPa Connect the carrier gas To do this connect...

Страница 42: ...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 fingers might be crushed Maintain a safety distance from th...

Страница 43: ...ect the other end of the data cable to the interface on the autosam pler Plug the grounding conductor into the connection on the rear of the analyzer Connect the supplied waste hose to the wash cup of...

Страница 44: ...changing the configuration Switch on the analyzer Start the multiWin program and initialize the analysis sys tem Check the device configuration with the Instrument System Information menu op tion in...

Страница 45: ...analyzer 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 M...

Страница 46: ...or CLD pump connection on the analyzer Connect the CLD HT interface on the rear of the analyzer with the RS 232 interface on the detector via the supplied serial data cable Switch on the detector The...

Страница 47: ...ule to the CLD pump connection on the rear of the analyzer Connect the connection hose for oxygen to the gas supply pressure reducer and to the oxygen gas connection on the rear of the solids module S...

Страница 48: ...on tube filled with catalyst 4 Gas outlet for measuring gas Sample supply The solids module has a furnace lock with interlock The furnace lock is mounted on the side opening of the combustion tube The...

Страница 49: ...lass when heating the combustion furnace This reduces the service life of the combustion tube Avoid touching the cleaned combustion tube with your hands during filling Wear protective gloves Only fill...

Страница 50: ...t then point downward Tighten the screws Close the furnace lock again Mount the module on the analyzer as follows Remove the combustion tube for vertical operation Remove the sealing plug from the hor...

Страница 51: ...FAST connector Screw the other hose 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 integra...

Страница 52: ...s use analytically pure acid HCl 2 mol l and make it out of con centrated acid and TOC water For TIC detection only use orthophosphoric acid H3PO4 10 made from concen trated acid p a and TOC water Sol...

Страница 53: ...er as follows Open the valve on the pressure reducer of the gas supply Switch on the PC Switch on the other optional components Switch on the analyzer via the main switch The status LED on the left fr...

Страница 54: ...Exit in the software interface The Program End window opens For measurements with autosampler Activate the Rinse syringe checkbox The sy ringe is flushed with the solution from the wash cup Activate t...

Страница 55: ...ld Enter the number of calibration points in the Number of standards input field Select the analysis parameters of the loaded method to calibrate in the Analysis pa rameters field Activate the IC and...

Страница 56: ...alibration tables are automatically assigned the kaltab file extension and are stored under Calibration Tables Click the Start measurement button Carry out the software instructions that follow Depend...

Страница 57: ...alculated concentration and the target concentration Linear Regression Qua dratic Regression Depending on the selected method the software calculates the regression formula and the method characterist...

Страница 58: ...easurement with the same method When the measurement is complete select the calibration report with the Add measuring point Add the new measuring points indi vidually to the calibration The software r...

Страница 59: ...ng calibration ranges Delete the calibration range Accept the current calibration data with Accept values Three calibration ranges exist A maximum of three calibration ranges can be stored for each pa...

Страница 60: ...he window with the Configuration Edit options menu option Export to clipboard Reopening a calibration report Click on the Data Evaluation CalibrationReport menu option in the main screen Select the ca...

Страница 61: ...the syringe canula up to the union nut The sep tum seals the system during injection Flip the lock switch to the rear Insert the syringe with septum far enough into the lock for the septum to seal the...

Страница 62: ...ampler can automatically acidify samples for NPOC measurement To do this fill the acid container with HCl 2 mol l Place the acid container at the acid po sition of the sample tray Start the measuremen...

Страница 63: ...ness of cleaning processes with swabs The swab can be tempered on a boat before wiping The blank value of the swab material can also be deter mined and taken into account Fold the swab using a pair of...

Страница 64: ...le boat in the solids module For multiple determinations Start a second measurement with new sample material by clicking Start At the end of the measurement the results appear in the analysis report o...

Страница 65: ...e electrochemical NO detector ChD optional in the right side part of the analyzer Sample supply system and autosampler Maintenance interval Maintenance task Quarterly Check the locks for leaks Every 1...

Страница 66: ...essary Replace a worn sealing ring of the lock Chemiluminescence detector CLD Maintenance interval Maintenance task Every 12 months Replace the adsorber cartridge 6 2 Adjustment and setting 6 2 1 Adju...

Страница 67: ...window tab Ana lyzer components with the Configuration Edit options menu option Select the syringe volume in the Syringe group in the Size list The syringe volume is specified on the syringe Click OK...

Страница 68: ...1 mm increments to align the piston position Move the syringe piston 2 down in steps until the slit is just no longer visible Start the adjustment of the syringe piston by clicking the Position Pisto...

Страница 69: ...Time field in the 1 to 900 s range For sample feed with autosampler In the Rack position field select any position on the sample tray to monitor the purge flow at Place a sample vessel with ultrapure...

Страница 70: ...TIC lock not relevant for multi N C 2100S pharma Septum on the dosing syringe of the autosampler with the septum free TC lock Replace the septums as required but at least after 12 months Replacing the...

Страница 71: ...been replaced 6 4 Replacing the pump hose CAUTION Risk of chemical burns during hose replacement Small quantities if acidic solutions can still be in the hoses Wear protective gloves and clothing when...

Страница 72: ...ill 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...

Страница 73: ...or operation 6 5 Replacing the hose connections FAST connectors connect hoses with glass components Use the threading aid to feed thin hoses into the connectors This is included with the analyzer Chec...

Страница 74: ...se with the conical side towards the banjo bolt The conical nipple and hose end must be flush Do not jam the banjo bolt during insertion and only tighten it hand tight 1 2 3 Figure 37Replacing the Fin...

Страница 75: ...e easy and difficult to oxidize such as sucrose and p benzoquinone Dispose of the catalyst in accordance with disposal regulations See also 2 Disposal 104 6 7 1 Removing the combustion tube CAUTION Ri...

Страница 76: ...s the pressure ring and the union nut from the com bustion tube Remove the used catalyst filling Check the combustion tube for heavy crystallization cracks and burst spots Only re use intact combustio...

Страница 77: ...z glass 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 th...

Страница 78: ...into the combustion tube easily Insert the rolled up HT 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 T...

Страница 79: ...top opening of the combustion furnace Insert the combustion tube into the combustion furnace Screw the lock loosely into the holder with the hexagon socket screw Hold onto the combustion tube at the...

Страница 80: ...ion again 6 8 Removing and installing the combustion furnace 6 8 1 Removing the combustion furnace CAUTION Risk of burns at the hot furnace Switch off the device and allow it to cool before performing...

Страница 81: ...led head screws Tighten the knurled head screws finger tight Plug the plug in connector for the combustion furnace into the socket at the bottom right of the rear device wall Install the combustion fu...

Страница 82: ...pply on the pressure reducer in the laboratory Open the left side wall of the analyzer Push the accessory modules to the side if necessary Do not kink any connection hoses Unscrew the four attachment...

Страница 83: ...arrier plate of the TIC condensate container and the condensa tion coil out of the mounting bracket on the right side of the furnace Pull hoses 1 16 and 21 with FAST connectors off of the connections...

Страница 84: ...ion into a beaker Check the TIC condensate container and condensation coil for deposits and cracks Rinse both glass parts with ultrapure water and dry it well Installation Slide the rubber ring onto t...

Страница 85: ...ds to the phosphoric acid pump Slide the two FAST connectors at least 1 cm onto the glass connec tions Attach the carrier plate to the mounting bracket on the right side of the furnace The spherical j...

Страница 86: ...e screws in turns Open the gas supply 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 10 Re...

Страница 87: ...sol 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 o...

Страница 88: ...Disconnect 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...

Страница 89: ...ect 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 th...

Страница 90: ...essary 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...

Страница 91: ...on 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 f...

Страница 92: ...which 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 re...

Страница 93: ...s 10 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 directo...

Страница 94: ...code 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 C...

Страница 95: ...bustion tube 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 rep...

Страница 96: ...The CLD detector is not switched on The connection cable is not connected or is faulty Incorrect connection Switch on the detector Check the connection cables Check the connection Error code Error me...

Страница 97: ...pair Error code Error message Minimum sample volume cup volume Cause Remedy For sample supply via autosampler Selected sample volume too large Number of determinations too high Check the following set...

Страница 98: ...y No carrier gas The hose line is leaking Turn on the carrier gas on the pressure reducer Search for and remedy the leak The inlet pressure of the carrier gas sup ply is too low Set the carrier gas in...

Страница 99: ...nalytic problems lead to implausible measurement results If the suggested solutions do not eliminate the errors problems and if such problems occur frequently contact the customer service department o...

Страница 100: ...in Fill the syringe with 0 1 n HCl Acting time 10 min Flush the syringe thoroughly with ultra pure water between cleaning steps and after cleaning Error Carry over Cause Remedy Insufficient syringe fl...

Страница 101: ...sample concentration is above the calibrated range Observe the calibrated range Use quadratic regression If possible calibrate dependent on the matrix For analysis of unknown substances use low concen...

Страница 102: ...o the canula The septum seals the lock during injection Lightly press the syringe onto the lock during injection Check the measuring gas flow in the Sys tem state window during injection Only remove t...

Страница 103: ...on LED strip not lighting Cause Remedy Incorrect temperature settings in the software Check the temperature settings under Configuration Options in the Analyzer components tab Faulty thermocouple furn...

Страница 104: ...will 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 requi...

Страница 105: ...injury 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 transpo...

Страница 106: ...screw in the screws on the bottom side and then on the top side Tighten the screws in turns Position the top furnace cover and secure it with adhesive tape Close the front doors of the analyzer Carefu...

Страница 107: ...isk of device damage due to environmental conditions Environmental influences and condensation can destroy individual components of the device Only store the device in air conditioned rooms Ensure tha...

Страница 108: ...ange 0 to 30000 mg l TC TOC in solid measurement range with the HT 1300 solids module 0 to 500 mg Nitrogen detection Nitrogen detection principle optional CLD ChD TNb measurement range CLD 0 to 200 mg...

Страница 109: ...ng altitude max 2000 m Control computer minimum re quirements Processor Disk drive RAM Screen resolution Min 3 2 GHz Min 40 GB Min 4 GB Min 1280 x 780 USB port Min 1 USB 2 0 interface for connecting t...

Страница 110: ...35 EU and 2014 30 EU The device leaves the factory in a sound condition with regard to technical safety To maintain this condition and to en sure safe operation the user must strictly observe the safe...

Страница 111: ...nges 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...

Страница 112: ...es 38 Figure 20 Device rear 40 Figure 21 Fasten the autosampler on the analyzer 43 Figure 22 Inserting the syringe 43 Figure 23 Chemiluminescence detector CLD 45 Figure 24 Connections on the backplate...

Страница 113: ...multi N C 2100S duo pharma Table of figures 113 Figure 41 Replacing the adsorber cartridge 92...

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