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Analysis

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3.2 TIC-determination

3.2.1 TIC-module

Due to the modular design of the CS-580 (Helios), the analyzer can be upgraded
by a module for Total Inorganic Carbon (TIC) without further modification. For the
TIC determination, the sample is treated with acid in the TIC module.

3.2.2 TIC analysis

The sample is treated with acid in an Erlenmeyer flask inside the TIC-module. The
acid decomposes the carbonates in the sample, creating CO2. The oxygen flow
purges the CO2 out of the flask through the gas flow system to the infrared
detector.

Fig. 7: Installation of TIC-module

Fig. 5: TIC-module

1

TIC module

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Содержание CS-580A

Страница 1: ... Eltra GmbH 42781 Haan Retsch Allee 1 5 Germany 02 07 2014 0001 Operating Manual Carbon and Sulfur Analyzer CS 580A Helios Original ...

Страница 2: ...2 Copyright Copyright by Eltra GmbH Haan Retsch Allee 1 5 D 42781 Haan Federal Republic of Germany ...

Страница 3: ...3 ...

Страница 4: ... the sample 18 3 2 TIC determination 19 3 2 1 TIC module 19 3 2 2 TIC analysis 19 3 2 3 TIC module installation 20 3 2 4 TIC module Operation procedure 21 3 3 Applications 22 3 3 1 Coal 22 3 3 2 Calcium Carbonate 22 3 3 3 Graphite 22 3 3 4 Limestone 22 3 3 5 Oil Asphalt and Rubber 22 3 3 6 Wood 22 4 Maintenance 24 4 1 General information 24 4 2 Reagent tubes filling 26 4 2 1 Reagent tube replacing...

Страница 5: ...4 Left side view inside 44 6 5 Furnace side inside view 46 6 6 TIC module 48 6 7 Packaging 50 7 Pre installation guide 51 8 Approved methodologies to which Eltra instruments conform 52 8 1 Inorganic materials Metals 52 8 2 Organic materials Oil Coal foodstuffs 53 9 Disposal 54 10 Index 55 Appendix following page ...

Страница 6: ... you the following warnings and corresponding content WARNING Type of danger personal injury Source of danger Possible consequences if the dangers are not observed Instructions on how the dangers are to be avoided We also use the following signal word box in the text or in the instructions on action to be taken WARNING Moderate or mild injury may result from failing to heed these safety warnings W...

Страница 7: ...property damage Source of property damage Possible consequences if the instructions are not observed Instructions on how the dangers are to be avoided We also use the following signal word in the text or in the instructions on action to be taken NOTICE ...

Страница 8: ...s an example of installation Fig 1 Arrangement Suggestion The environment of the device does not have to necessarily be air conditioned although it is best if the room temperature remains between 18 C and 30 C NOTICE Under no conditions the device should be placed in direct sunshine Avoid places exposed to the wind of air conditioners or to the wind blowing through open windows or doors 0 1 2 3 C ...

Страница 9: ...eter 8 Carrier gas flow meter 9 Lance flow meter 10 Lance flow adjustment 11 Furnace low inlet 12 Dust filter cartridge 0 1 2 3 C S Analyser Auto sampler Air Power Inlet Gas P r e c l e a n i n g Carrier M o i s t u r e t r a p HELIOS 8 0 2 0 1 2 0 A i r 2 0 C 1 0 1 3 2 5 P a l h 2 0 0 5 0 3 0 0 A i r 2 0 C 1 0 1 3 2 5 P a l h 2 0 0 1 0 0 5 0 3 0 0 A i r 2 0 C 1 0 1 3 2 5 P a l h Inlet Lance 1 0 0...

Страница 10: ...t standby position 1 during working breaks to keep the IR cell operating temperature stable The furnace temperature is software controlled Fig 2 Rearview Mains power connections 1 Analyzer 2 Computer 3 Monitor 4 Printer 5 Balance 6 Quad power socket At first only the analyzer 1 is plugged in and switched on Turn the mains power switch to position 1 stand by condition The switch is on the front pan...

Страница 11: ...ntroller board 1 PC USB connector 2 Power and temperature control interface 3 Analog input output signals 4 Pump control 5 24V connector 6 Digital input output signals 7 Autoloader connection 8 Regulating valve not relevant for CS 580A When all units are connected to the mains power then interface connections can be made The required interface cables are included in the scope of supply The supplie...

Страница 12: ...side of device Tube 1 connects the oxygen supply to the analyzer on the fitting of a pressure regulator This connection must be very secure considering that the incoming oxygen pressure in the tube is 2 to 4 bar 30 to 60 psi Do not tighten the nut too much in order to avoid damaging of the tube Drive the cup nut manually Don t use any tool Fig 2 Compressed air connection The tube 2 connects the de...

Страница 13: ...moisture which has entered the gas flow system can be purged by the oxygen flow Keep it there for about 10 15 minutes before starting the first analysis To save time the purging can be started before the set temperature has been reached The slight influence of the oxygen flow on the temperature of the infrared cell is compensated At short working breaks like lunch breaks the mains switch remains o...

Страница 14: ...eter 8 Carrier gas flow meter 9 Lance flow meter 10 Lance flow adjustment 11 Furnace low inlet 12 Dust filter cartridge 0 1 2 3 C S Analyser Auto sampler Air Power Inlet Gas P r e c l e a n i n g Carrier M o i s t u r e t r a p HELIOS 8 0 2 0 1 2 0 A i r 2 0 C 1 0 1 3 2 5 P a l h 2 0 0 5 0 3 0 0 A i r 2 0 C 1 0 1 3 2 5 P a l h 2 0 0 1 0 0 5 0 3 0 0 A i r 2 0 C 1 0 1 3 2 5 P a l h Inlet Lance 1 0 0...

Страница 15: ...y the customer as needed During heating up to the set temperature the ceramic combustion tube is under high thermic stress This stress is increased with increasing speed of the heating up process For maximum service life of the combustion tube the furnace can be heated up slowly with a heating rate of 10 C min In order to avoid long waiting time until the furnace heats up the heating up of the fur...

Страница 16: ...artup menu of Windows This enables the start of the UNI software with every start of the PC The shortcut is deleted automatically when the preheating is deactivated 2 9 2 BIOS configuration In order to start the preheating before the work begins the BIOS has to be configured to start the PC automatically at the selected time The preheating starts automatically by starting the UNI software 1 Switch...

Страница 17: ...to the crucible 4 Press the F4 Balance button in the Analysis control window of the software or F4 on the PC keyboard to transfer the weight value from the balance to the PC The transfer function is performed regardless how often the button is pressed This enables a correction of any falsely entered weight 5 Enter the sample ID into the corresponding input field of the Analysis control window of t...

Страница 18: ...sis control window of the software This step is optional If no sample ID is required the entry may be omitted Press the F2 Furnace button to open the furnace if it is closed Take the crucible from the balance and put it on the pedestal Press the F5 Start button to begin the analysis From now on no further operator intervention is required The furnace closes and the analysis is carried out automati...

Страница 19: ...n For the TIC determination the sample is treated with acid in the TIC module 3 2 2 TIC analysis The sample is treated with acid in an Erlenmeyer flask inside the TIC module The acid decomposes the carbonates in the sample creating CO2 The oxygen flow purges the CO2 out of the flask through the gas flow system to the infrared detector Fig 7 Installation of TIC module Fig 5 TIC module 1 TIC module ...

Страница 20: ...f the analyzer and of the TIC module 4 The outlet of the furnace is connected via the H2O trap to the connection 2 and finally to the inlet 1 of the TIC module 5 Inside the TIC module this tube is connected to the input of the glass distributor 3 connection on top tube 4 6 The bottle of acid with dispenser 9 is placed to the right of the platform 8 and it is connected to the connection 5 of the gl...

Страница 21: ...t the flask so that its bottom lies flat on the heated platform 6 Switch to TIC mode with the TIC TC toggle 13 7 Start analysis F5 or click START 8 Inject acid in two or three doses when the word Analyzing appears 9 When all the CO2 has been released from the sample the analyzer s signal will return to the baseline level and the analysis will be terminated 10 switch to TC mode with the TIC TC togg...

Страница 22: ... 3 1 Coal Temperature 1350 C Weight 300mg 500mg Depending on the sensitivity of the IR cell and on the C and S content of the sample No accelerators are needed Only in exceptional cases when the sample contains pyrites the furnace temperature has to be set at 1500 C or approx 300mg of iron phosphate have to be spread on top of the sample 3 3 2 Calcium Carbonate NOTICE Calcium carbonate can be used...

Страница 23: ...Analysis 23 Weight 350mg Set the minimum analysis time to 50s Set the comparator level to 20mV ...

Страница 24: ...with the moisture The saturation of the sodium hydroxide changes its color it turns to light grey The magnesium perchlorate is saturated if its particles do not move when tapping on the glass tube It is essential to change the absorber before it becomes cloggy The moisture absorber should be checked every 100 200 induction analyses and if necessary it should be replaced glass tube underneath the m...

Страница 25: ...fect and affects repeatability Another typical effect is that the analysis takes too long and it is often not even completed This effect also occurs with magnesium perchlorate of suitable quality when it is saturated The commonly available sodium hydroxide binds CO2 very inadequately at room temperature whereas the special quality not only perfectly binds CO2 at room temperature but also contains ...

Страница 26: ... are fitted both the O rings and the inner ends of the tubes are lubricated with high vacuum silicon grease The components are refitted in reverse order NOTICE The dimensions for filling the glass tubes should be respected in all cases to secure proper analyzing and to avoid any damages of the device see chapter filling quantities When there is not enough glass wool in the lower end of the glass t...

Страница 27: ...erial A clear sign of total saturation is when the absorber s particles do not move freely after tapping at the glass tube Normally the moisture absorbers should be checked after 30 to 40 analyses The grade of the absorber saturation is at its maximum at the gas entrance of the tube and it becomes gradually less toward the glass tube outlet Therefore once the upper half only of the magnesium perch...

Страница 28: ... 4 Empty 5 Sodium hydroxide 90210 0 1 2 3 C S Analyser Auto sampler Air Power Inlet Gas P r e c l e a n i n g Carrier M o i s t u r e t r a p HELIOS 8 0 2 0 1 2 0 A i r 2 0 C 1 0 1 3 2 5 P a l h 2 0 0 5 0 3 0 0 A i r 2 0 C 1 0 1 3 2 5 P a l h 2 0 0 1 0 0 5 0 3 0 0 A i r 2 0 C 1 0 1 3 2 5 P a l h Inlet Lance 1 0 0 4 0 F i l t e r 35 15 65 4 2 1 20 90 25 90 25 1 5 1 2 1 ...

Страница 29: ...the glass tube 5 Remark The O ring imprint on the whole circle length of the glass tube should be of about 2 mm width 4 4 O rings replacing The O rings are only replaced when they no longer adequately seal due to severe damage or aging When removing the old O rings be sure that the sealing area of the fittings is not damaged Grooves where the old O rings are installed must be cleaned to be complet...

Страница 30: ...n the sample material and its combustion characteristics The filtering material of a new cartridge is white Replace the dust filter cartridge when the filtering material shows coloration or at least every 500 analysis Fig 12 Dust filter cartridge inserting 1 Lift the dust filter cartridge 1 upwards 2 Tilt its low end to the front and pull downwards 3 Install a new cartridge by acting in reverse or...

Страница 31: ...ains power plug before opening the analyzer s cabinet Fig 7 Removing the combustion tube Switch off the analyzer and disconnect the power plug Remove the cover panel 1 of the cabinet Unscrew 4 screws 2 on top Remove the tubes 3 4 and 5 from the upper furnace closure assembly 6 7 Remove the 4 screws 8 which hold the assembly 6 7 on the furnace The 4 screws and nuts holding the disk 7 on the part 6 ...

Страница 32: ... driven screws 13 Lift the combustion tube 12 out of the furnace top Lift it in straight vertical direction to avoid collision with the heating elements Place a new O ring 9 on a new combustion tube 12 Reinstall in reverse order NOTICE Enter the new combustion tube very carefully in straight vertical direction to avoid collision with the heating elements 4 7 Lance replacing DANGER G0002 Mortal dan...

Страница 33: ...re opening the analyzer s cabinet Fig 9 Operating procedure for replacement of heating elements Remove the combustion tube See chapter Combustion tube replacing Remove the two screws 1 fixing the right hand side panel 2 of the analyzer s cabinet Slightly tilt the panel to the right and carefully lift it The loader should not be shifted otherwise it will lose its mechanical adjustment Unscrew the t...

Страница 34: ...heating elements 15 Reinstall in reverse order using new heating elements Remark Install the clamps 14 in a position which allows the heating elements to move at least 5 mm in vertical axial direction Insert the thermocouple deep enough to touch the combustion tube and fix it with the spring ...

Страница 35: ...re that a dry dust free gas mixture is supplied to the infrared cells The output signals of the infrared cells are selective and correspond to the SO2 and CO2 concentrations in the gas mixture They are electronically linearized integrated divided by the sample weight and displayed as S and C values Since the sample weight is taken into account the results don t depend on the sample weight For this...

Страница 36: ...18 Gas flow meter 5 Oxygen stop valve software controlled 19 Infrared cell 6 Flow adjustment restrictor 20 Gas flow meter 7 Carrier gas flow meter 21 Attenuator before the pump 8 Gas pre cleaning unit 22 Gas flow pump 9 Oxygen diverting valve 23 Attenuator after the pump 10 Flow adjustment restrictor 24 Microcontroller 11 Gas flow meter 25 Computer 12 Upper furnace closure assembly 26 Monitor 13 F...

Страница 37: ... help of the adjustable restrictor 6 the inlet flow is set at a level of at least 200 l h The flow rate is shown on the lower flow meter 7 on the front panel This flow rate enters the furnace During analysis when the furnace is closed the inlet flow rate is split One part enters the furnace top to exit the lance over the crucible This flow is shown on the middle flow meter 11 The rest of the oxyge...

Страница 38: ...Function description 38 Fig 14 Gas flow ...

Страница 39: ... leaves the IR path it passes through an infrared filter which allows only a certain narrow band infrared radiation to pass This narrow band must correspond to the IR wavelength for which the gas to be detected has its maximum absorption capability The intensity of the radiation after the filter thus corresponds to the concentration of a specific gas in the path The beam finally strikes a solid st...

Страница 40: ...beginning of the combustion and it ends after a pre set minimum time In case the combustion takes longer the integration is prolonged Then the detector signal is compared to a comparator level The integration continues as long as the IR output signal is higher than the comparator level When it comes down below this level the integration is stopped Should the IR signal remain above the comparator l...

Страница 41: ...ive reagent tube with bigger capacity 09093 Alternative reagent tube with maximum capacity 11170 Dust filter cartridge 11480 Adjustable restrictor 15087 Flow meter 300l h 15095 Flow meter 600l h 36700 Upper reagent tube holder 36710 Lower reagent tube connector 48067 Lower reagent tube connector 48069 Upper reagent tube connector 70320 O ring ...

Страница 42: ... air 78017 Mains power switch 6 2 Rear side outside view Fig 11 Rear side inside view Part Nr Description 14618 Microcontroller board UNI 1 4 15268 Pump control boart PC1 35490 Pump support 15270 Gas pump 35325 Attenuator volume 35336 Attenuator volume 35456 Blower 60234 Pneumatic valve 60522 Fitting 90 ...

Страница 43: ...552 Adjustable restrictor 77032 Circuit breaker 77140 Mains power filter 77145 Mains power filter 77460 Switch 6 3 Bottom outside view Fig 12 Bottom view Part Nr Description 11035 Cooling fan 11492 Oxygen pressure regulator ...

Страница 44: ...1492 35526 35537 60353 Sensor 16114 PTC2 36915 78072 3 4 1 2 Relay RC Bu1 77051 35533 77052 11480 1 0 5 2 1 5 A i r 2 0 C 1 0 1 3 2 5 P a l h 15083 11490 36284 36284 26320 26320 36914 MD50 35779 78051 FD15 Digital I O Loader Power temp control Analog I O Microcontroller board UNI 2 1 Part No 18468 Regulating valve PC Pump control 24VDC 78052 16114 35779 18468 FD37 06441 ...

Страница 45: ...NI2 26320 Insulator 35536 2 2 way valve 24VDC 35779 Power temperature control cable 36284 Heating element connector 36798 Transformer 36904 Temperature control board TH 44 36914 Thermocouple 36915 Power temperature control board 60353 Piston sensor 77051 Thyristor block 77052 Solid state relay 78051 Pump control cable 78052 USB cable for PC interface 78072 Current transformer ...

Страница 46: ...e view Fig 13 Furnace inside view inside Part Nr Description 35408 Lower plate insulation 35462 Upper plate 35512 Ceramic plate 35540 Combustion tube 35541 Ceramic lance 35542 Pedestal 36284 Heating element connector 36289 Heating element clamp ...

Страница 47: ...Ordering numbers 47 70150 O ring 70427 O ring 70428 O ring 77501 Heating elements 4pcs 77505 Ceramic spacer 90150 Crucible ...

Страница 48: ...Ordering numbers 48 6 6 TIC module Fig 17 TIC module 35543 9008 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 ...

Страница 49: ...50 ml glass flask 90090 7 Heater with magnetic stirrer 71070 8 Support with variable height 38400 9 O ring 9 3 70230 10 Lower moisture trap connector 11045 11 Geared mechanism 38850 12 Glass stopper connection to the furnace 38227 13 Glass stopper connection to the acid supply 38220 14 Glass support 38340 15 Dispenser Assimat 71065 16 Acid bottle 71060 17 Bottle support 38677 ...

Страница 50: ...here the analyzer is put on is very important It should neither be too hard nor too soft When the foam is too soft the analyzer will practically touch the wood Fix the foam on the bottom of the wooden case by gluing The small loader with 36 trays can be packed in the wooden case together with the analyzer The bigger loaders for 104 and 130 crucibles however are to be packed in separate carton boxe...

Страница 51: ...imension 850 x 350 x 450mm depending on version Analyser weight approx 90kg Loader weight approx 55kg The balance should rest on a vibration free support Loader dimensions Version 36p 500x250x460mm Version 130p 900x500x460 Gas connections The supplied tubes carry a connector with G inner diameter Fig 15 Carrier gas tube Connections for compressed air The tubes supplied together with the analyzer c...

Страница 52: ...el Iron Nickel Cobalt Alloys CS 800 CS 2000 ON 900 OH 900 ONH 2000 ASTM E 1587 2010 C N O S Refined Nickel CS 800 CS 2000 ON 900 OH 900 ONH 2000 ASTM E 1409 2013 N O Titanium and Titanium Alloys ON 900 OH 900 ONH 2000 ASTM E 1569 2009 O Tantalum ON 900 OH 900 ONH 2000 ASTM E 1937 N Titanium and Titanium Alloys ON 900 ONH 2000 ASTM E 1447 2009 H Titanium and Titanium Alloys OH 900 ONH 2000 ASTM E19...

Страница 53: ...1552 2008 S Oil and Petrolium Products CS 580 CS 2000 ASTM D 4239 2013 S Coal and Coke CS 580 CS 2000 ASTM D 5016 2008 S Coal and Coke Ash CS 580 CS 2000 ASTM D 1619 2011 S Carbon Black CS 580 CS 2000 PN G 04514 17 1993P S Coal and Coke CS 580 CS 2000 DIN EN 13137 2001 12 C Waste CS 580 CS 2000 DIN ISO 10694 1996 08 C Soil samples CS 580 CS 2000 ...

Страница 54: ...nal provisions that are based on the EU Directive 2002 96 EC on Waste Electrical and Electronic Equipment WEEE Accordingly all machines supplied after 13 08 2005 in the business to business area to which this product is classified may no longer be disposed of with municipal or household waste To document this they have the following label Fig 18 Disposal label Since the disposal regulations within...

Страница 55: ...CS 580A front view 40 D Data Interface 11 Disposal 53 Disposal label 53 dividing 39 Dust filter cartridge inserting 29 Dust filter cartridge replacing 29 E Explanations of the safety warnings 6 F Figure Dust filter cartridge inserting 29 Filling quantities 26 Front panel illustration 9 Function description 34 Furnace side inside view 45 furnace temperature 15 G G 50 Gas connections 50 Gas flow 37 ...

Страница 56: ...gen connection 12 P Packaging 49 Preheating the furnace 15 Pre installation guide 50 property damage 6 R Reagent tube replacing 25 Reagent tubes Installalling 25 replacing 25 Reagent tubes filling 25 Rear side outside view 41 Rear side inside view 41 rear side of device 12 Rearview Mains power connections 10 S Safety warnings 6 sample materials 34 serious injury 6 service manual notes 6 Setting ch...

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Страница 60: ...Copyright Copyright by Eltra GmbH Haan Retsch Allee 1 5 D 42781 Haan Federal Republic of Germany ...

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