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Endress+Hauser Analytik Jena TOPwave Operating Manual Download Page 57

TOPwave 

Operating 

 

 

57 

 

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Summary of Contents for Analytik Jena TOPwave

Page 1: ...Operating Manual TOPwave Microwave System for Pressure Digestion...

Page 2: ...1 07745 Jena Deutschland Telefon 49 3641 77 7407 Fax 49 3641 77 7449 E mail service analytik jena de Follow these instructions for proper and safe use Keep for future reference http www analytik jena...

Page 3: ...4 6 Operating 27 6 1 Setup Methods 27 6 1 1 General Notes 27 6 1 2 Control Unit 28 6 1 3 Selecting modifying Applications 29 6 1 4 Developing new Applications 32 6 2 Performing a Digestion Procedure 3...

Page 4: ...ips and Tricks 74 11 1 1 Small sample quantity 74 11 1 2 Multiple samples per vessels 74 11 1 3 Higher sample throughput 74 11 1 4 Cooling down samples 75 11 1 5 Dilating Sealing lips 75 11 1 6 Ruptur...

Page 5: ...l word The type source and consequences of the danger are stated together with notes on preventing the danger The meaning of the signal words used is explained in section Safety instructions p 8 The e...

Page 6: ...re and temperature conditions in chemical la boratories Digestion is understood to mean the decomposition of a solid material by means of a suitable digestion reagent at increased temperature in a ves...

Page 7: ...t unauthorized alterations or modifications by qualified users Please also observe all regulations published by professional trade associations the T V VDE regulations or corresponding national regula...

Page 8: ...safety and environmental protection must be observed and complied with References to potential dangers do not replace the work protection regulations which must be observed 2 1 1 Safety information on...

Page 9: ...ndling of chemicals Prohibited for persons with heart pacemakers WARNING The microwave device must not be operated by persons with heart pacemakers 2 3 Safety instructions transport and commissioning...

Page 10: ...be immediately returned to Analytik Jena for inspection Never attempt to use force to open the vessels Never use tools to open the vessels The pressure vessels are equipped with a rupture disc which...

Page 11: ...supply Renew vessels WARNING Renew the vessels after around 10 000 digestions to maintain reliable operating condi tions and to prevent negative influences on your analysis results e g memory effects...

Page 12: ...ugh this PFA vent tube WARNING Hot acid vapors may be released The supplied vent tubes must therefore always be properly connected and attached to an exhaust system Make sure the PFA tube is securely...

Page 13: ...h Load bearing capacity min 80 kg 176 lb Electrical connection 230 V 50 60 Hz Ventilation slots at the rear must be free minimum distance 15 cm Make sure that the TOPwave microwave system is set up an...

Page 14: ...and regulated is integrated in the microwave oven The measurement physi cally determines the temperature radiation emitted by the vessel contents that is the digestion solution Radiation components e...

Page 15: ...3 Vent connection oven 6 Electrical connections The electrical connections are located on the right hand side of the microwave system 1 Power switch 3 Connection power cord 2 Fuses 4 RS 232 port The m...

Page 16: ...digestion process data The last data file is displayed in example above Data ddir1_0 Logged in Display of login status After pressing the line the login window appears Open Release the electronic lid...

Page 17: ...mperatures below 50 C 122 F are indicated on the display by low 1 Infrared filter 2 Measurement sensor 4 3 Pressure Monitoring Option Optionally TOPwave can be equipped with a pressure monitoring syst...

Page 18: ...disc activates are guided to a collection system integrated in the rotor Thereby the va pors are vented or suctioned off through the PFA tube connected to the swiveling lid PM 40 vessels are made enti...

Page 19: ...PTFE insert 8 pressure vessels made of TFM PTFE 8 pressure vessels made of TFM PTFE with RPM For the digestion of smaller sample quantities the QX 20 quartz glass inserts can be in serted into the PM...

Page 20: ...uantities of samples or several samples simultaneously in a PL 100 or CX 100 pressure vessel The vessels for the MT system are made of PFA have a capacity of 10 ml and a graduation mark at 5 ml see se...

Page 21: ...ec tion If it is necessary to use an extension cord to connect the system to the power supply only a three wire cord with a ground connection may be employed The unit should not be set up near any dev...

Page 22: ...ivates NOTICE Provide a suitable vent Users are responsible for assuring that appropriate ventilation of toxic gases is assured Make sure that all ventilation procedures conform to applicable laws Use...

Page 23: ...r switch 2 Mains connection 3 Fuses 4 USB port 5 RS 232 port 6 Ethernet port Switch the TOPwave on and wait 5 seconds before switching on the control unit at mains power switch and wait until the Logi...

Page 24: ...he red handle The lid then swings to the right to its end stop After 10 seconds the lid is automatically locked again In this case again press O PEN The rotor for the pressure vessels is preassembled...

Page 25: ...appears Is OFF displayed the Main menu will be shown off off on PRESSURE ON OFF The OPC pressure measurement can generally be activated or deacti vated off off on MAX DIGESTION TIME Max runtime of a t...

Page 26: ...Installation and Setup TOPwave 26 The TOPwave is now ready for operation...

Page 27: ...imarily carbon dioxide generated by samples containing carbon also produce pressure This pressure is therefore dependent on the sample amount the vessel volume as well as the carbon content of the sam...

Page 28: ...rupturing pre maturely 6 1 2 Control Unit The control unit is operated via a touch screen In order to trigger a function briefly press on the representative symbol on the screen Pressing OK or ESC alw...

Page 29: ...s 25 of which are preinstalled After accessing the APPLICATION function initially a selection of maximally 12 appli cations is displayed which the user can compile to form a User Library Favorites Fur...

Page 30: ...ngth of time in minutes required to heat to the target temperature Permitted values 0 59 min TIME Display and input of the length of time in minutes for which the target temperature is to be kept cons...

Page 31: ...ters see above With SAVE EXIT confirm the changes and return into the Main menu The changed application is used for the next digestion Of the 200 applications in the selective list 30 are pre installe...

Page 32: ...evant technical literature for a corresponding process instructions For safety reasons first reduce the specified weight of the samples by 30 50 in terms of the maximum permissible sample weight for t...

Page 33: ...ot gases and vapors may be released from the digestion vessel when it is opened Al ways make sure the vent opening on pressure vessels faces away from both yourself and other individuals Only open the...

Page 34: ...ad can also result in rotor overheating and in the worst case in rotor damage Visually inspect the rupture discs In case of extensive traces of corrosion or other visible damage to the rupture discs t...

Page 35: ...s a fume hood WARNING Hot acid vapors may be released The supplied vent tubes must therefore always be properly connected and attached to an exhaust system Make sure the PFA tube is securely attached...

Page 36: ...n this window you can select a file name create a new file or reset the index num ber For selecting a file mark the correspondent line in the list and press NEXT For creating a new file enter the file...

Page 37: ...view of all vessels Select with the buttons and the vessel for displaying curves The vessel is marked in the bar graphs Target temperature and pressure are displayed in the field SET Actual temperatur...

Page 38: ...r volumes of liquid must be used at least 3 vessels must be used for each run in order to achieve the required total load If the fluid amount employed is too small the oven may be damaged during longe...

Page 39: ...lge in the center of the rupture disc after use is normal and will not affect its functions Make sure the rupture disc is properly seated in the locking lid that is that its edge sits uniformly in the...

Page 40: ...fter weighing in the sample material and adding the acid the locking lid is pressed on whereby resistance should be clearly felt If this is not the case the sealing lip must again be dilated as descri...

Page 41: ...e vent fitting onto the associated collection vessel tube it may be necessary to first move the vessel into the proper position 1 Vent fitting 2 Vessel tube Seal any unused positions on the collection...

Page 42: ...ration An inadequate liquid load can also result in rotor overheating and in the worst case in rotor damage The procedure for the quartz glass inserts QX 20 QX 22 with pressure vessels PM 60 PL 100 i...

Page 43: ...ON Rupture discs and pressure vessels Observe the safety instructions in the sections Safety instructions p 8 and Performing a Digestion Procedure p 33 Never use more than one rupture disc per vessel...

Page 44: ...t be dilated again as described above The locked TFM liner is now inserted into the CX 100 pressure digestion vessel toge ther with the ceramic pressure jacket The titanium rupture disk is now placed...

Page 45: ...tools to open the vessels The pressure vessels are equipped with a rupture disc which produces a spontaneous pressure release upwards through the screw on tube connections in case of excessive vessel...

Page 46: ...t only the bases of the vessels come into contact with the cooling water A total cooling time of at least 20 minutes is required for these vessels To open the vessels hold onto the coupling cap and sl...

Page 47: ...ly for each vessel and if need be saved after digestion has been completed Prior to saving the index of the data file is automatically incremented Press the DATA button in the Main menu for displaying...

Page 48: ...ge The selected point in time is shown on the left below The target temperature and the pressure are displayed in the field SET Temperature and pressure of the selected vessel are displayed in field b...

Page 49: ...the stick copy all data from the control unit to the stick and remove the stick Observe all status signaling on the right above Observe that you can use only the same stick Switch off the control uni...

Page 50: ...0 0 0 0 0 0 0 0 0 0 50 90 34 95 95 95 95 95 95 95 95 95 95 95 95 95 50 155 14 50 0 0 0 0 0 0 0 0 0 0 0 0 0 0 50 90 34 95 95 95 95 95 95 95 95 95 95 95 95 95 50 155 16 50 0 0 0 0 0 0 0 0 0 0 0 0 0 0 50...

Page 51: ...tive gloves during work which may in volve contact with chemicals that is when working with acids pressure vessels during cleaning etc WARNING Hot acid vapors are generated Risk of acid burn Hot acid...

Page 52: ...oning Aside from the requirements cited in the Ambient Conditions p 13 section the opera tion of the gas scrubber also requires a coolant water connection approx 0 5 li ters min with an inlet temperat...

Page 53: ...ys wear safety glasses goggles and protective gloves during work which may in volve contact with chemicals that is when working with acids pressure vessels during cleaning etc After the samples have b...

Page 54: ...am typical values 5 10 C The magnetron temperature is recorded conti nuously and is used to control the distillation process The terminate criterion is met if in step 5 the magnetron temperature rises...

Page 55: ...tion vessel This liquid must be removed after every fuming procedure see section Cleaning p 61 All TFM PTFE components must be cleaned with water and dried before they are again used 6 8 PC Control Op...

Page 56: ...our Administrator to obtain these On no account should you alter the Ethernet settings of your PC Software requirements Java must be installed correctly http java com Microsoft Internet Explorer or Mo...

Page 57: ...Properties with a right click on the adapters used Local Area Connection Properties window appears Select Internet Protocol Version 4 TCP IPv4 and confirm by using the Properties button Confirm Inter...

Page 58: ...f the control system as a trusted site in the Internet browser Internet options trusted sites Here explained by means of the Microsoft In ternet Explorer 10 Select the Trusted sites in the Security ta...

Page 59: ...ct visualization the control system must be switched to opera tion with Web Visualization in the Setup menu For this purpose you set WEB VISU to ON The following safety warning indicates that Java has...

Page 60: ...curity warning appears Click on Run to start the application 6 8 4 Data transfer To open the SD card folder via the FTP server the following address must be en tered ftp root root 192 168 0 199 You wi...

Page 61: ...pres sure vessels Note any changes in the appearance of the pressure vessel which could indicate possible material fatigue e g deformation of the vessel difficulty screwing on lids etc even when the...

Page 62: ...with cleansing wipes or a sponge can be recommended or a subsequent com plete digestion with a suitable acid mixture The glass rings installed in the cap for pressure control have to be cleaned from t...

Page 63: ...rt on the pins of the assembly stamp Put the coupling cap on the cap insert and press the cap on Rotate the assembly stamp in a position that the connecting fitting can be screwed in Screw in the conn...

Page 64: ...m Only then remove the protection foil from the over side of the polarization foil Cut off remains with a sharp knife or scissors Insert the glass prism into the copling cap und fix it see above For a...

Page 65: ...be occasionally replaced Unscrew the fixation screw on the collection vessel Exchange the lip seal for a new one Fasten the fixation screw finger tight again 1 Fixation screw 2 Lip seal 3 Collecting s...

Page 66: ...the rate at which it heats becomes significantly slower To measure the output power 500 ml water is heated at full microwave power for 42 seconds and then the rise in temperature established The outpu...

Page 67: ...ax 30 minutes Spark formation in the oven Acid volume too low Rupture disc corroded or da maged Increase quantity of fluid refer to Operation minimum filling quantity Exchange burst disk Exhaust air t...

Page 68: ...defective Replace Rupture disc more frequently Check turntable function Reduce weighing in quantity Reduce maximum tempera ture Contact Service Rupture disc trigger frequently applies to RPM pressure...

Page 69: ...wave Maintenance 69 NOTICE Use only OEM fuses in accordance with the description below Fuse Type Size 20 x 5 mm 250 VAC 12 5 AT If the fuses again trip after being replaced inform the Service Departme...

Page 70: ...e must be brought to the appropriate waste disposal center for cor rect disposal according to the appropriate legal guidelines At the end of its service life the TOPwave and all its electronic compone...

Page 71: ...s Weight approx 65 kg 143 lb without vessels Noise level 60 dB DIRC temperature range 50 C 300 C 122 F 572 F Pressure sensor range 0 150 bar 2180 psi Display 0 100 bar 1450psi dependent on used vessel...

Page 72: ...PL 100 100 ml 40 bar 580 psi 210 C 410 F 500 mg 7 ml CX 100 100 ml 100 bar 1450 psi 250 C 482 F 1000 mg 7ml QX 20 QX 22 20 ml 100 bar 1450 psi 230 C 446 F 300 mg 7 ml Material TFM PTFE quartz aluminum...

Page 73: ...tive 2014 35 EU Electromagnetic Compatibility Directive 2014 30 EU for device security RoHS Directive 2011 65 EU on the restriction of the use of certain hazardous sub stances in electrical and electr...

Page 74: ...ity of the TOPwave to be raised Cross contamination from one sample to another is prevented by pre filling the same acid mixture into the outer vessel as in the inner vessel If the acid volume on the...

Page 75: ...fers TFM PTFE caps with the PM 60 and PL 100 vessels which are used without additional metallic rupture disks Potential applica tions are for example digestions for ultra trace analytics such as those...

Page 76: ...sample and remain there during digestion Since the vessels exhibit prac tically no memory effects the cleaning process is the same as in the case of the digestion vessels 11 2 Applications A multitude...

Page 77: ...n Sample number Rotor position 2 1 2 3 4 5 6 7 8 9 10 11 12 8 1 2 3 4 5 6 7 8 9 10 11 12 3 1 2 3 4 5 6 7 8 9 10 11 12 9 1 2 3 4 5 6 7 8 9 10 11 12 4 1 2 3 4 5 6 7 8 9 10 11 12 10 1 2 3 4 5 6 7 8 9 10...

Page 78: ...2 5 1 5 7 3 8 4 6 2 11 4 Conversation of units Temperature C F F 32 1 8 1 8 C 32 Length 1 cm 1 inch 0 3937 inch 2 540 cm Volume 1 ml 1 inch3 1 gallon 0 06102 inch3 2 642 10 4 gallon 16 387 ml 43 29 1...

Page 79: ...e Appendix 79 11 5 Abbreviation Abbreviation Technical term PE Polyethylene PEEK Polyetheretherketone PFA Perfluoralkoxy PTFE Polytetrafluorethylene TFM PTFE Modified Polytetrafluorethylene PP Polypro...

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