Endress+Hauser Analytik Jena TOPwave Скачать руководство пользователя страница 6 | Manualshive

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Endress+Hauser Analytik Jena TOPwave Скачать руководство пользователя страница 6

Basic information

TOPwave

6

The following signal signs are used in the manual!

WARNING

Warning of dangerous explosive substances!

WARNING

Warning of dangerous electrical voltage!

1.2

Intended Use

WARNING

The unit is not designed for extraction and metabolization procedures employing orga-

nic solvents.

WARNING

Since sample composition is generally not precisely defined, a certain residual risk exists
when performing pressure digestion processes. Careful working practices and conscious

compliance with safety regulations can only minimize this risk, not totally eliminate it.

Due to different degrees of mixing, even identical samples can exhibit totally different
behaviors during the course of the reaction!
Please strictly comply with the operating instructions, particularly when handling the

pressure vessels, that is, when removing and opening the vessels. Incorrect handling of
the hot, pressurized vessels can result in injuries from escaping acid vapors!

The TOPwave microwave digestion system has been designed to perform chemical di-
gestion procedures under extreme pressure 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 vessel that is per-
meable with regard to microwaves. The digestion solutions are directly heated through

the absorption of the microwave radiation by the polar digestion reagent, which gene-

rally also contains ionic components.
Digestion reagents used include nitric acid (65 %), hydrochloric acid, hydrofluoric acid,

phosphoric acid, and sulfuric acid, as well as mixtures of these acids. The maximum ini-

tial weight for organic compounds depends on the digestion vessel being used and the
sample’s carbon content, must always be observed. The use of organic solvents is strictly

prohibited in microwaves since the spontaneous combustion of any solvent vapors that

escape into the oven chamber cannot be precluded.
Heating in the pressure vessel results in digestion temperatures in excess of 200 °C

(392 °F). The TOPwave has been specially developed for sample preparation for AAS

and ICP spectroscopy procedures. Very temperature spikes >280 °C (>536 °F) such as can
occasionally occur during the course of exothermic reactions can result in irreversible da-

mage to the Teflon vessels.

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Содержание Analytik Jena TOPwave

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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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