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Operating instructions

1. _ FRITSCH 11 Exclusion of liability Before using the product be sure to have read and understood this operating manual The use of the product requires technical knowledge only commercial use is permitted The product may be used exclusively within the scope of applications set down in this operating manual and within the framework of guidelines put forth in this operating manual and must be subject to regular main tenance In case of non compliance improper use or improper mainte nance the customer assumes full liability for the functional capability of the product and for damage or injury arising from violating these obliga tions The contents of this operating manual are subject in entirety to copy right law This operating manual and its contents may not be copied fur ther distributed or stored in any form in part or in whole without the prior written consent of Fritsch This operating manual has been prepared to the best of our knowledge and checked for accuracy at the time of printing FRITSCH GMBH assumes no guarantee or liability whatsoever for the accuracy or com pleteness of the contents of this operating manual including but not limited to the implied warranties of merchantability and fitness for a par ticular purpose unless liability is expressly prescribed by applicable laws or jurisprudence FRITSCH GMBH expressly reserves the right to modify and or update this operating manual without prior notice
2. IT FRITSCH A 5 6 4 Number and size of the balls Pre grind course hard material with large balls reduced percentage of fine material Many small balls increase the percentage of fine material during extended running time 5 6 5 Weight of the balls type of material A higher mass specific weight of the grinding balls accelerates grinding see table in Choice of grinding bowls and grinding balls on page 31 5 7 Dry grinding Below a particle size of approx 20 um the surface forces prevail The grinding stock begins to stick Additional dry comminution can be achieved by adding surface active substances to the material to be ground Examples maximum amount to be added in mass Stearic acid 2 3 Aerosil fine particle silicic acid 0 5 2 Quartz sand 2 Glass powder 2 Glycol Ethylene glycol 0 1 0 5 4 5 25 droplets Triethanolamine 0 1 0 5 5 8 Wet grinding grinding in a suspension A DANGER Explosion hazard Ignition hazard The device is not explosion protected If flammable liquids are used make sure that the heat developing in the grinding bowl does not reach the solvent s boiling point Program appropriate cooling phases If the vapour pressure is too high vapours may escape and ignite If it can be avoided we recommend using non flammable liquids or liquids with a high boiling point The boiling point should be above 80 C and above 100 C for
3. Generally applicable legal and other obligatory regulations regarding environmental protection must be observed 1 4 Information on hazards and symbols used in this manual Safety information Safety information in this manual is designated by symbols Safety infor mation is introduced by keywords that express the extent of the hazard DANGER This symbol and keyword combination points out a directly hazardous situation that can result in death or serious injury if not avoided WARNING This symbol and keyword combination points out a possibly hazardous situation that can result in death or serious injury if not avoided CAUTION This symbol and keyword combination points out a possibly hazardous situation that can result in slight or minor injury if not avoided NOTICE This symbol and keyword combination points out a possibly hazardous situation that can result in property damage if not avoided Special safety information To call attention to specific hazards the following symbols are used in the safety information 10 FRITSCH Safety information in the procedure instructions DANGER This symbol and keyword combination points out a directly hazardous situation due to electrical current Ignoring infor mation with this designation will result in serious or fatal injury DANGER This symbol and keyword combination designates contents and instructions for proper use
4. Press the Load button to transfer the program data record 3 Press the lt button to return to the main menu The program is disabled by manual input e g of the speed see amp Program sequence after switching on on page 50 55 FRITSCH u 5 12 7 Setting the time control 1 p Select Menu 2 p Select Clock 3 p Select the time base for the internal clock 4 Press the lt button to confirm your entry 56 FRITSCH u 5 Enter the time offset By entering a time offset grinding is only started after this delay in time This function is displayed as active in the main menu 6 Press the lt button to confirm your entries gt The time offset is reset to 0000 after grinding 5 12 8 Imbalance check The distribution of different weights in both bowls will obviously result in different vibrations also depending on the speed To tolerate this imbalance within specific limits you can set the shut down threshold 57 FRITSCH Unbalance control Switching off Touch the adjustment bar or move it back and forth by applying slight Pressure Press the lt button to confirm your entries Small setting values make the measuring system more sen sitive and high values make it less sensitive NOTICE If the permissible maximum temperature in the bowl is exceeded during grinding then the device must not be s
5. ee ee eee 38 114 FRITSCH a ei FRITSCH u 2012 Fritsch GmbH Milling and Sizing Industriestra e 8 D 55743 Idar Oberstein Telephone 49 0 6784 70 0 Fax 49 0 6784 70 11 Email info fritsch de Internet www fritsch de
6. The same applies to modifica tions and improvements to the products described in this operating manual It is the responsibility of the user to ensure that they have the current version of this operating manual For more information please contact your local FRITSCH GMBH distributor or Fritsch GmbH Industri estr 8 D 55473 Idar Oberstein Not all parts shown here are necessarily installed in the product The buyer is not entitled to delivery of these parts If interested please con tact your local FRITSCH GMBH distributor or Fritsch GmbH Industriestr 8 D 55743 Idar Oberstein FRITSCH GMBH takes the greatest care to ensure that the quality relia bility and safety of your products are continuously improved and adapted to the state of the art The supplied products as well as this operating manual conform to the current state of the art when they leave the sphere of influence of FRITSCH GMBH By using the product the customer agrees with this and recognizes that defects malfunctions or errors cannot be completely excluded To pre vent risk of damage to persons or property or of other direct or indirect damage resulting from this or other causes the customer must imple ment sufficient and comprehensive safety measures for working with the product 109 zu FRITSCH Fritsch GmbH excludes any liability warranty or other obligation to com pensate for damages regardless of whether this liability warranty or ot
7. button to save your entry and return to the main OD vi menu 01 Off 12 Press the Start button to close the grinding chamber cover and start the safety check 0400 010 13 Various sensors check the bowls and the closing mechanism That will take a few moments Berns Shutter closed Cup locked X Mee es 295 FRITSCH A meene 14 The sensors detect that the grinding bowls are not present Shutter closed x a 15 Press the gt button to open the grinding chamber cover and a BR onal rinding station 1 is moved into the loading position Cup locked x Failure R 16 The device functions are OK 4 3 Switching off If the device is put out of service for a lengthy period close the grinding chamber cover using the Close button and turn the device off at the main switch 26 FRITSCH 5 Using the device 5 1 Safety information A DANGER The PULVERISETTE 7 premium line planetary mill from Fritsch enables speeds of up to 1100 rpm The application of high energy may result in very high temperatures and high pressures in the grinding bowl Failure to observe the following safety instructions could result in the explosion of grinding bowls and parts flying around causing injuries and damage to the building or device We cannot accept any liability for the occurrence and con sequences of injuries or damage to the building or device
8. references and other elements the following designations are used in this manual Designation Explanation Step by step procedure instructions 1 233 ey Results of steps in the procedure hy References to sections in this manual and rele vant documentation a Lists without a specific order Button Operating elements e g push button switch display elements e g signal lamps Display Screen elements e g buttons function key assignment 12 1 5 Information on hazards at the device FRITSCH A There is a laser radiation hazard warning on the back of the device It is explained below Do not remove the information and warning signs Caution Hot surface Caution Crushing hazard 1 6 Device safety information BE Only use genuine accessories and genuine spare parts Failure to observe this instruction can compromise the safety of the machine E Accident proof conduct is to be strictly followed during all work 135 FRITSCH DANGER Explosion hazard Wear safety goggles The high temperature or chemical reactions during the grinding process may result in overpressure in the grinding bowl Splashing hazard Explosion hazard Do not fail to observe amp Safety information on page 27 and Safety measures against an excessively high pressure on page 40 Never use brute force to open the grinding bowl Open the grinding bowl only if you are sure that the interna
9. 20 45 80 volume ml 20 Number of balls St 5 15 Number of balls St 7 10 10 Number of balls St 10 18 25 30 5 Number of balls St 80 180 250 Ball with a diameter of 3 mm and smaller Material Grinding bowl 20 45 80 volume ml Zirconium oxide Amount of balls 30 70 100 grams Tempered steel Amount of balls 40 90 150 grams Tungsten carbide Amount of balls 80 200 300 grams eye FRITSCH A 5 2 4 Calculated weight of a ball Ball diameter in mm 5 10 15 20 Material Density Calculated weight of a ball in g in g cm Agate 2 65 0 17 1 39 4 68 11 1 Silicon nitride 3 25 0 20 1 16 5 48 12 99 Sintered 3 9 0 25 eis 6 72 15 92 corundum Zirconium oxide 57 0 37 2 98 10 07 23 88 Stainless steel 7 8 0 51 4 08 13 78 32 67 Tempered steel 7 9 0 52 4 14 13 96 33 09 Tungsten car 14 9 0 96 7 40 25 98 61 58 bide To determine the weight of the required balls the calculated weight of a ball is multiplied with the amount of balls required Example A 45 ml agate bowl is to be filled with 185 agate balls with a diameter of 5 mm Calculation 0 17 g x 185 St 31 45 g 31 45 g grinding balls can be weighed and inserted in the grinding bowl thus avoiding the time required for counting the balls 5 3 Impact of the ball size and the material during grinding Large balls with a diameter of 10 mm 20 mm will result in high mechanical system stress The combination of the heavy weight of the balls and high acc
10. 60 6 1 Standard gassing lid for grinding with inert gas 60 6 1 1 Scope of delivery uuessnssseeeenensneesnnenennennennneennnnnennenn nenne 60 6 1 2 Fitting the gassing lid on the grinding bow 61 FRITSCH A a 6 1 3 Hose adapter for grinding bowl gassing 63 6 1 4 Removing the gassing lid in individual steps 64 6 2 Gassing lid with stainless steel swagelok hose couplings 66 6 2 1 Scope of delivery lid DeSIgN ccccccccceesseeeeseeseeeeeeeees 67 6 2 2 Fitting the gassing lid on the grinding bow 67 6 2 3 Hose adapter for grinding bowl gassing 69 6 2 4 Removing the gassing lid in individual steps 70 6 3 EASY GTM Gas Pressure and Temperature Measuring SVS p A A S A E EE 71 6 3 1 Case contents and system Ce SIEN ccccceeeeeseceeeeeeeneees 72 6 3 2 Inserting changing the battery ccccccccccesseeseeeeeeees 72 6 3 3 Configuration of transmitter ID and data transmission EE E ee a 75 6 3 4 Installation of the transmission unit on the EASY GTM DOW ee ee A N 76 6 3 5 Installation of the receiver board in the P 7 premium ee ee 78 6 3 6 Activating EASY GTM cc csssssscccceecceesseeceeeeseeeeeseeeeeeeees 79 6 3 7 Entering the temperature limit ss222200022enee een 81 6 3 8 Entering the pressure limit cccccc
11. The same applies to dry grinding with less than the minimum sample quantity NOTICE If the minimum filling quantity is fallen short of increased wear due to abrasion is to be expected This can cause irreparable damage to the mill components 36 FRITSCH A 5 5 Filling the grinding bowl Do not fail to comply with the following sequence 1 Place the grinding balls in the empty bowl 2 Fill material to be ground over the balls CAUTION Never operate the device without material to be ground otherwise the grinding balls and grinding bowl will be dam aged 5 6 Factors with an impact on grinding 5 6 1 Running time grinding duration 5 6 2 Speed 5 6 3 Reverse mode A longer grinding duration will increase the percentage of fine material To reduce the running time you can use a grinding bowl and grinding balls with a higher density and thus a higher impact energy Higher speeds shorten the grinding time and increase the share of fine particles NOTICE The grinding duration in the reversing mode must not exceed 5 minutes A longer grinding duration in the reversing mode may damage the PULVERISETTE 7 premium line Useful for mechanical alloying Improvement of the homogeneity of the sample The grinding duration of a grinding cycle in reversing mode must not exceed 5 minutes The overall duration is determined by the number of cycles Overall grinding duration time x cycles
12. a long grinding duration 38 _ FRITSCH During the transition to grinding in suspension you can add a liquid aux iliary agent with high boiling point and low vapour pressure e g water white spirits boiling point 100 140 C or alcohols with a high boiling point e g isopropanol We recommend that you only use so much liquid that the suspension has the same consistency as motor oil With this viscosity the best results can be achieved in most cases 5 8 1 The effect of high temperature DANGER During wet grinding in the grinding bowls the high internal temperature the increase in size of the surface of the parti cles due to crushing and any chemical reactions in the bowl may result in the development of a very high pressure This pressure can get so high that the hooks that hold the lid on the bowl crack resulting in the lid flying off During grinding tests chemical reactions of steel parts tempered steel and stainless steel and tungsten carbide parts with water suspension were determined After a grinding period of 20 minutes the increase in pressure could tear off the locking hooks The grinding bowl temperature may be rela tively low DANGER Explosion hazard Ignition hazard Burn hazard In the event of a longer grinding duration apply cooling pauses to reduce the internal pressure For certain material to be ground it may also be necessary to release the pres s
13. amp Standard Operation Proce dure on page 94 please contact the PULVERISETTE 7 administrator This mode must be deactivated otherwise only programs already stored can be loaded for operation To activate the EASY GTM system proceed as follows 79 FRITSCH u 1 p Select Menu 2 Select EasyGTM sub menu 3 gt Activate EASY GTM 4 The inverted button indicates the current status 80 FRITSCH 6 3 7 Entering the temperature limit 1 Select the maximum temperature input If the max temperature is reached the device stops the grinding process and goes into cooling mode p Depending on the setting of the operating mode see amp Selecting the operating mode on page 83 the device stops the grinding process and opens the grinding chamber cover or reduces the speed gradu ally until a minimum speed is reached in order to ach ieve an optimal cooling effect 2 Enter the required max temperature limit DANGER Do not exceed a maximum temperature of 125 C Other wise the EASY GTM system and the machine will be dam aged 3 Use the lt button to confirm your entry and return to the EASY GTM sub menu 4 Select the minimum temperature input When the selected min temperature e g 60 C is reached again during the cooling phase the mill starts the grinding process again 5 Enter the required min temperatur
14. and the suspension from the device after grinding and remove the lid amp Opening the grinding bowl after a grinding operation on page 41 87 2 Fit the adapter 6 with stainless steel strainer 4 and seals 2 5 7 firmly on the grinding bowl and tension it like a lid amp Closing the grinding bowl on page 42 FRITSCH A 3 Screw on the funnel lid 2 for holding the syringe on the adapter 6 4 Fill the syringe 1 with 10ml air 5 Screw the syringe 1 onto the funnel lid 2 of the special emp tying device 6 Inject the air in the syringe 1 into the bowl 88 FRITSCH A 7 _ Shake the bowl with the suspension 8 Pump 2 5 times with the syringe and then mount the syringe 1 9 Now the suspension is in the syringe 10 Unscrew the syringe 1 from the funnel lid 2 11 Solvent can again be injected into the bowl using the emptied syringe to extract the last remains of the sample Repeat the pro cedure 5 to 10 times 12 Open the system by turning the funnel lid 2 down and separate the adapter 6 by pushing the locking hooks off the grinding bowl 13 The suspension is in the syringe and the balls are lying on the stainless steel strainer 4 89 FRITSCH A 6 4 3 Cleaning the special emptying device 6 5 Compl counterweight It is cleaned under running water To do this remove all
15. bit 7 Hexagon offset screwdriver 2 5mm 2 2x battery 1 5 V AA 8 Measuring transmission unit 3 EASY GTM system 9 Lid 4 Flat sealing ring 54x2 silicone foam 10 Compl bowl 5 O ring 21x2 5 11 locking ring with 6 socket head screws 6 Hexagon screwdriver 3mm 6 3 2 Inserting changing the battery Prior to initial start up the battery 2 provided must be inserted in the measuring transmission unit 8 of the system When inserting it for the first time and during subsequent replacement of the battery proceed as follows 7 FRITSCH A 1 If not already done switch off the radio system using the button A The LED B goes out 2 Then release the six socket head screws C for closing the system using a hexagon screwdriver 7 The locking ring 11 with 6 socket head screws can be removed now see Cleaning the EASY GTM system on page 84 3 Carefully lift the measuring transmission unit 8 off the bowl 10 4 Ifthe lid 9 is on the unit release it by hand and place it to the side The lid normally remains on the bowl 10 In FRITSCH A 5 Undo the two screws D of the battery compartment using a hex agon offset screwdriver size 2 5mm 6 6 Lift off the battery compartment lid and place it to the side The battery compartment can be seen NOTICE Please note that the the battery 2 fits exactly in place and may need to be pushed in using a
16. by those responsible for the safety of the machine to carry out the required work and are able to recognize and avoid possible hazards as defined for skilled workers in IEC 364 In order to prevent hazards to users follow the instructions in this manual Malfunctions that impair the safety of persons the PULVERISETTE 7 pre mium line or other material property must be rectified immediately The following information serves both the personal safety of operating per sonnel as well as the safety of the products described and any devices connected to them All maintenance and repair work may only be per formed by technically qualified personnel This operating manual is not a complete technical description Only the details required for operation and maintaining usability are described Fritsch has prepared and reviewed this operating manual with the greatest care However no guarantee is made for its completeness or accuracy Subject to technical modifications The planetary micro mill PULVERISETTE 7 premium line can be applied universally for the fast dry or wet grinding of inorganic and organic sam ples for analysis quality inspection or material testing During the synthesis the planetary micro mill is for mixing and homoge nising dry samples emulsions or suspensions The planetary micro mill PULVERISETTE 7 premium line described here is an equipment item for use in industrial environments The device may be used for
17. line gradually reduces the speed down to a minimum speed If these two limit settings are fallen short of significantly the device accelerates back to the operating speed Stop As soon as one of the two limits is reached the ball mill shuts down immediately If the limits are fallen short of restart is disabled Press the lt button to confirm all entries and return to the main menu 6 3 10 Deactivating EASY GTM To deactivate the EASY GTM system proceed as follows 1 Select Menu 2 Select EasyGTM sub menu 83 3 gt Deactivate EASY GTM FRITSCH A 4 Press the lt button to confirm your entry and return to the main menu 6 3 11 Cleaning the EASY GTM system NOTICE The threaded holes inside the bowl the passage holes and the Allen screws in the locking ring have to be cleaned thor oughly after each grinding to allow a safe fastening of the EASY GTM system NOTICE The measuring transmission unit 8 may not be immersed in water It can be rubbed down with a damp cloth if neces Sary Remove the locking ring including the screws of the measuring transmis sion unit and clean it completly The screws are provided with a snap ring which prevents them to fall out of the locking ring Pay attention to the position of the snap rings see picture 84 d socket head screws FRITSCH A When inserting the locking ring 11 make sure th
18. of the machine in explosive areas or with explosive substances Ignoring information with this designation will result in serious or fatal injury DANGER This symbol and keyword combination designates contents and instructions for proper use of the machine with com bustible substances Ignoring information with this designa tion will result in serious or fatal injury WARNING This symbol and keyword combination points out a directly hazardous situation due to movable parts Ignoring infor mation with this designation can result in hand injuries WARNING This symbol and keyword combination points out a directly hazardous situation due to hot surfaces Ignoring informa tion with this designation can result in serious burn injuries due to skin contact with hot surfaces Safety information can refer to specific individual procedure instruc tions Such safety information is embedded in the procedure instructions so that the text can be read without interruption as the procedure is being carried out The keywords described above are used sifa FRITSCH A Example 1 gt Loosen screw 2 p CAUTION Risk of entrapment at the lid Close the lid carefully 3 Tighten screw Tips and recommendations This symbol emphasises useful tips and recommendations as wells as information for efficient operation without mal function Further designations To emphasise procedure instructions results lists
19. permitted mass differ ence depends on various parameters like rotational speed or stability of the substructure Basically the lower the rotational speed the higher the mass difference can be 5 11 Grinding duration Depending on the application the grinding duration should be adapted to the development of heat of the bowls When grinding at high speed a grinding duration of 1 hour depending on the temperature should not be exceeded Then allow the unit to cool down for half an hour to an hour If a chemical reaction takes place in the grinding bowl the result may be the development of a very high pressure in the grinding bowl without the temperature exceeding 100 C The pressure must also be released when the grinding bowl has cooled down The PULVERISETTE 7 premium line is not suitable for grinding with steel or tungsten carbide grinding bowls in water suspensions The application of extremely high energy results in abrasion wear in the nano range That can result in chemical reactions that cannot be controlled 6 To what extent the heating up of the material to be ground needs to be observed naturally depends on the corre J sponding sample in each individual case Note gt a longer duration may also require a long pause time for cooling down 48 FRITSCH A 5 12 C If bowls are removed during a grinding pause check that the bowl is seated correctly before the device is switched back on Cond
20. result from errors at installation improper opera tion or improper use or improper maintenance or are in any way con nected to these 110 FRITSCH uf 12 Safety logbook Date Maintenance Repair Name Signature 111 FRITSCH a EEE Date Maintenance Repair Name Signature 112 FRITSCH 13 Index A Accident prevention 0000s 8 Activating EASY GTM nern 79 Activating SOP mode 2 00 eee ene 95 Adjustment options of the transmitter detection 75 Ambient conditions 2 22 2222er 22 Authorised persons 22222222 eee eens 8 B Batteryarrangement 2222er 86 C Case content EASY GTM wid ee oS eae oe rue 72 Cleaning Grinding elements 22222 104 Menere rns eree es eeute ee eae e Bees 104 the special emptying device 90 Cleaning the EASY GTM system 84 Cleaning the sensor 0 02 eee ee eee 85 Closing the grinding bowl 0 42 Conduction of a grinding operation 49 Configuration of transmitter ID 75 Cooling the grinding bowl 59 Counterweight 0 eee eee eee eee 90 Current consumption 0 02 00 18 D Deactivate bowl detection 4 97 Deactivating EASYGTM 2 2222202 83 Deactivating SOP mode 222222 95 Deleting SOP mode 2 222 96 Design of a grinding bowl 22222 41 of the counte
21. 1 Hexagon socket wrench 13mm 5 2 x valve inserts replacement 2 2x flat seal 57 5x48x2mm silicone for grinding bowl 6 Valve key for turning the valve inserts out of the 1 x replacement valve 3 Compl gassing lid 7 Hose with adapter on valve 4 4x flat seal 6 3x1 8x1mm viton for valves replace ment 60 6 1 2 Fitting the gassing lid on the grinding bowl FRITSCH A 1 Place the silicone flat seal 2 on the edge of the bowl insert 9 Gassing lid handle 2 The central handle 9 must be removed as illustrated 3 Hold the lid at the hook Push the hook up and place the lid on the bowl 4 Turn the lid with the hooks pressed outwards on the bowl until the lugs of the hooks engage in the recesses on the edge of the bowl fitting amp Closing the grinding bowl on page 42 61 5 After releasing the hooks they must be immersed completely in the recesses on the outer diameter of the bowl fitting and be exactly vertical FRITSCH A 6 Push the central handle 9 down by hand until the resistance increases 7 _ Use the hexagon socket wrench 1 to tighten it with maximum manual force The maximum manual force is equivalent to a torque of approx 3 5 4Nm iG FRITSCH nm 8 This is what the closed grinding bowl looks like 6 1 3 Hose adapter for grinding bowl gassing m x 5 1 Push the locking lev
22. 4 Turn the lid 2 on the bowl until the small lugs a of the locking hooks 4 engage in the recesses on the edge of the bowl 5 Release the locking hooks 4 and push them together at the bottom end until they engage and are exactly vertical ee FRITSCH A 6 Make sure that the locking hooks engage exactly in the middle of the recess Only then can the bowl be closed properly and inserted in the device r Make sure that the distances are the same 7 _ Turn the handle 5 down firmly the press on sleeve 7 must be released for air to escape from the bowl 8 Turn the press on sleeve 7 down firmly NOTICE Once the locking hooks are engaged the lid may no longer be turned against the bowl The positions of the hooks and grooves in the bowl below the hooks must match 5 9 4 Inserting the grinding bowl in the grinding bowl holder Carry out the following checks before inserting the grinding bowls 1 Are the grinding bowls clean on the outside gt remove any coarse dirt 2 Is the grinding bowl adapter clean on the inside gt remove any coarse dirt 3 Are the grinding bowls sealed correctly see Using the device on page 27 Inserting the grinding bowls A4 1 Open the clamping bracket 10 FRITSCH A 10 Clamping bracket 11 Locking element 12 Bracket guide 2 Hold the grinding bowl at the handle 5 and set it in the grinding
23. F second ON OFF 4 second OFF ON automatic ON ON 1 second transmission is the default value For automatic transmission the 1 second transmission frequency is switched over in the event of fast changes in pressure or temperature The data transmission frequency naturally also has an impact on the bat tery s service life 1 second operation results in the longest time span The transmission frequency can also be checked visually as soon as the transmission unit is switched on the switch flashes each time data is transmitted 6 3 4 Installation of the transmission unit on the EASY GTM bowl NOTICE The threaded holes inside the bowl the passage holes and the Allen screws in the locking ring have to be cleaned thor oughly after each grinding to allow a safe fastening of the EASY GTM system The EASY GTM system must be assembled as follows before inserting the EASY GTM system in the micro mill I6 FRITSCH A 1 Insert the seal in the bowl 2 Insert the intermediate lid NOTICE Always insert the intermediate lid before grinding with the EasyGTM system Fritsch assumes no guar antee for damage caused by grinding without the intermediate lid 3 Apply the transmitter with seal 4 Tighten the socket head screws crosswise with a torque spanner 1 until it disengages To be on the safe side re tighten all screws again after initially tightening them All sc
24. H A 5 1 2 Overpressure relief of the grinding bowls The grinding bowl seals have a sealing effect but are also for overpres sure relief If the pressure increases gradually during grinding the special seals open at a certain pressure and release the overpressure in a defined manner DANGER This overpressure release does not work in the event of sudden pressure surges e g explosions A half round notch with a diameter of 2 mm is punched onto the outer diameter of the flat seal The grinding bowl s pressure release works with flat seals made of fluororubber above a static internal grinding bowl pressure of about 10 bar Flat seals made of silicone open above a static internal grinding bowl pressure of about 18 bar DANGER If flat seals are used without this defined notch very high pressures will develop in the grinding bowl that could cause it to burst resulting in damage and injuries The application of high energy during grinding results in high tempera tures in the grinding bowl An 80 ml grinding bowl filled with 60 ml water results in the development of the following pressures and temperatures Temperature of grinding bowl Pressure in the grinding bowl wall C bar 101 1 109 2 127 4 141 6 152 8 159 10 166 12 171 14 177 17 180 19 183 21 If water is used as an additive the overpressure release with fluoror ubber flat seals is triggered at 159 C and with silicone flat seals at 180 C an An
25. ITSCH u 7 3 Language change After selecting the national language all other texts are displayed in the selected language Press the lt button to confirm your entry and return to the main menu 98 FRITSCH u 7 4 Screen brightness The screen s brightness can be adjusted individually To do this touch the adjustment bar or move it back and forth by applying slight pressure Press the lt button to save your entry and return to the main menu 99 FRITSCH u 7 5 Information The INFO button can be pressed to access system information operating hours the firmware version and the bowl materials are displayed here if they were detected during a START procedure Press the lt button to return to the main menu 100 FRITSCH zu 7 6 Interfaces In the standard case the device is equipped with a USB port lm An Ethernet or Bluetooth interface can be provided in the future as an option The interface selection must be switched over accordingly The optional interfaces have their own installation instructions within the scope of delivery Press the lt button to save your entry and return to the main menu 101 FRITSCH A 7 7 Firmware update Switch off the device Install the USB driver software PL 2303 Driver Installer exe on the PC notebook Connect the USB cable and only then
26. The display lights up 3 During the start and initialisation phase you can press the INFO button to have information displayed with the contact address Press the Next button to close this information again 4 Grinding station 1 is moved into the loading position The grinding chamber cover opens automatically 5 Insert the grinding bowl Filling the grinding bowl on page 37 loaded with the sample amp Handling the grinding bowl on page 41 and closed correctly in the grinding bowl holder Inserting the grinding bowl in the grinding bowl holder on page 44 Grinding station 1 is moved into the loading position The grinding chamber cover opens automatically Insert the grinding bowl Filling the grinding bowl on page 37 loaded with the sample amp Handling the grinding bowl on page 41 and closed correctly in the grinding bowl holder Inserting the grinding bowl in the grinding bowl holder on page 44 You can press the Close button c to close the grinding chamber Press the Next button b to return to the main menu 50 FRITSCH A Cycles O14 FT Revers Off 10 To enter the process parameters either press the indication d of the data touch function or press the MENU button e gt press the PARAMETER button f to open the parameter input screen 11 The field coloured in black is active When you start to enter a number th
27. _ FRITSCH Operating instructions PLANETARY MICRO MILL PULVERISETTE 7 premium line Valid starting with 07 5000 00100 Read the instructions prior to performing any task Translation of the original operating instructions FRITSCH a Fritsch GmbH Milling and Sizing Industriestra e 8 D 55743 Idar Oberstein Telephone 49 0 6784 70 0 Fax 49 0 6784 70 11 Email info fritsch de Internet www fritsch de Version 10 2013 Index 019 FRITSCH A Certifications and CE conformity Certification CE Conformity Fritsch GmbH has been certified by the TUV Zertifizierungsgemeinschaft e V TGA T LER PUR AT EIN GERMAN ASIOCIATION FOR ACCREDITATION OM Dh TGA ZM 05 08 00 An audit certified that Fritsch GmbH conforms to the requirements of the DIN EN ISO 9001 2008 The enclosed Conformity Declaration lists the guidelines the FRITSCH instrument conforms to to be able to bear the CE mark FRITSCH A Table of contents 1 Safety information and USEC cccccccsssecccesseecceeeeceeseseeeeaeaees 8 1 1 Requirements for the USEP ccccccseccccesceceseceeeseceeeceeenecs 8 1 2 Scope Of APPLiCAatiON ceccceesecccessececeseceeeeceeeeseceeeeeeeenees 8 1 2 1 Operating principle 9 1 2 2 Drive motor and speed regulation ccccccccsseseeeeeeeeees 9 1 3 Obligations of the operator uusssessennesnenennnennnnnennnenennnn 9 1 4 Inform
28. at the two holes are positioned over the socket head screws d The lid normally remains on the bowl 10 If the lid 9 is on the measuring transmission unit 8 release it by hand before cleaning The lid 9 and the bowl 10 can be cleaned under run ning water as described in amp Grinding elements on page 104 6 3 11 1 Cleaning the sensor and replacing the seal The sensor G must not be subjected to any mechanical stress It is per mitted to cleaning it with a wet cloth The O ring 5 can be replaced if necessary 85 FRITSCH A 6 3 12 Battery arrangement According to the DIRECTIVE 2006 66 EC OF THE EUROPEAN PARLIA MENT AND COUNCIL as of 6th September 2006 on batteries and rechargeable batteries and on old batteries and old rechargeable bat teries and for the annulment of Directive 91 157 EEC and article 1 18 and article 2 of the German Act on the re definition of the wast legisla tion on the product responsibility for batteries and rechargeable bat teries BattG as of 25 06 2009 we are legally obliged as the manufac turer to inform you as the consumer about the following The Easy GTM product we sell contains a lithium battery type AA 1 5V that can be discharged once When the battery is flat it may not be disposed of along with household waste Old batteries may contain harmful substances that can pollute the environment or damage your health Please deliver the batteries to
29. ation on hazards and symbols used in this manual 10 1 5 Information on hazards at the CeVICE cseccccseeeeeeeeees 13 1 6 Device safety INFOrMAtION ccccccessccceeeeeceeceeeeeceeeeeeeeees 13 1 7 Protective equipment 2ss02es0esonnnonnnnononnnnnnnnnnennnnennenn 15 1 8 Hazardous POINtS ccccsecccsececssecceseceeeeceeeneeceeceeeeceesneeeees 16 1 9 Electrical safe asirese aa E 16 1 9 1 General infOrmMation ccccccccccsscceseceeseeceeeeceeeeeneeeeneeees 16 1 9 2 Protection against restart s us2s02s0nsennennenennenenn nennen 17 1 9 3 Overload Protection cccccccscccccsseccceesceeeeceeeeeceseeeeeeees 17 1 94 Imbalancedelecetion eusussnneienein 17 2 Technical 033 need 18 2 1 DIMENSIONS anna 18 22 NO Eee ee ee 18 2 3 Operating No Se ee 18 2 VOTE Oe A EEE A AET 18 2 5 Curent conSsUMPEION een 18 2 6 Power CORSUMPLON en nanreeeeae 18 2 1 Eleetrical TWSES sionen 19 28 MAT ale ee 19 29 Fpa RINGING SS seeen en 19 3 Installation een 20 31 Trans pOl RENTE TEE PER SER PERDERRUISEURTEREHERUERVERUEPENEHRERIEE EIERN 20 32 UMD ACKING isviner ariei 20 3 3 SENE Ufer T 21 3 4 Ambient conditionS eeseesssesseessreessrresrressrrresereerrereerereererse 22 3 5 Electrical connection run 22 4 Initial Start Up ccccccceeccccceseccccsssecceaeseceeseeceeeeseeeseeeeeseagees 24 Ae SWEN Oietan a en EROA EITE 24 22 FURCHOMCHecK EEA 24 43 Switching Oft nenne 26 5 Usin
30. bowl adapter 3 Turn the grinding bowl until it can be felt to engage and drops a few millimetres into the grinding bowl adapter 4 Push the locking element 11 down on the bowl holder gt the grinding bowl is lowered within the mounting device AG FRITSCH A 5 Apply vertical pressure to the grinding bowl handle 5 to lock the grinding bowl in place in its adapter The grinding bowl is locked correctly if the locking element 11 on the mounting device moves back up into its initial position 6 Push the clamping brackets 10 down until they engage in the bracket guides 12 provided and can not be moved down any fur ther 7 _ As long as the locking element 11 and the locking brackets 10 are not in their original positions the rotation of the complete mill mechanism is blocked 5 9 5 Removing the grinding bowl 1 Open the clamping bracket 10 2 Push the locking element 11 down on the bowl holder AG 3 The grinding bowl is unlocked and moves up a few millimetres FRITSCH A 4 Now the grinding bowl can be removed upwards from its holder Hold the grinding bowl preferably at the handle 5 provided for this purpose 5 When the grinding bowl is removed the locking element 11 moves back into its initial position 6 Push the clamping brackets 10 down until they engage in the bracket guides 12 provided and can not be mov
31. can now be lifted off the pallet and out of the foam pad ding CAUTION Crushing hazard Always lift with 2 persons Hold the bottom edge of the housing when lifting E Compare the contents of the delivery with your order 20 FRITSCH A C Grinding bowls made of tempered steel may have recesses on the surface caused during production They do not have J an impact on grinding or the grinding results and usually disappear after the first grinding operation These recesses on the surface if present are within the range of the permissible production tolerances Complaints relating to such grinding bowls therefore cannot be accepted 3 3 Setting up E Set up the planetary micro mill indoors on a flat and firm surface NOTICE Never operate PULVERISETTE 7 premium line while it is standing on the transport pallet EB Make sure that all switches control elements are easy to access the ventilation slots are not covered the interfaces USB Ethernet are easy to access CAUTION Risk of overheating The cover on the housing openings may reduce the supply of air thus causing the device to overheat m Please store the transport packaging in order that it can be reused in case you need to return the product Fritsch GmbH denies all liability for any damage due to improper packaging non genuine packaging 21 FRITSCH A 3 4 Ambient conditions WARNING Mai
32. ceecceeeceeeeceeeeeeeeees 82 6 3 9 Selecting the operating MOE ccccseeeccesssseeeeeeeeeeeees 83 6 3 10 Deactivating EASY GIM cccccscccsscceseeeeeeceeceneeceseeeeaees 83 6 3 11 Cleaning the EASY GTM System ccccccsseeeeeeseeeeeeeees 84 6 3 12 Battery arrangeMent ccccsecssccsscssesssceecesscasceseeeeees 86 6 4 Special emptying device for grinding bowIs 86 DAT CSCI een 87 674 2 TOUS see ee ee 87 6 4 3 Cleaning the special emptying deVICE cceeceeseeeeees 90 6 5 Compl COUNTErWEIGNT ccccceccceeeceseceeeeceeeeceeeeeeeeneeeeess 90 Mc MSU e E secre ee 91 652 CHING ee nee 91 6 6 Planetary mills MillControl software 93 7 General and optional settings 22222222220002000n nennen 94 7 1 Standard Operation Procedure cccccccssseeeceesseeeeeeseeees 94 7 1 1 Activating SOP MOde ccccccccssssececcseseceeeeeeeecesseaesees 95 7 1 2 Deactivating SOP MOE cccccccsssseceeceeeseceeeeaeseeeeeeaeesees 95 7 13 Deleting SOP MORE are 96 VD Dee 97 7 3 Language CHANG ren een 98 7 4 Screen brightness ussscscneiecin nennen 99 7 5 HFORMaAHON a nein 100 7 8 IMEI ES ee ae are 101 77 Firmware update ee 102 FRITSCH A 10 11 12 13 CVO AINE essen nes nee een en 104 8 1 Grinding ClEMENTS cccccceeeccceesececeeeeceseeceseeneceeseeeesees 104 9 2 UN eases cape eee ee ee 104 8 2 1 Removing t
33. certain amount of force The service life of the battery 2 depends on the frequency of the radio protocols see configuration and essentially on the temperature inside the grinding bowl Also pay attention to the battery s charge level If the bat tery s capacity falls below 10 it should be replaced imme diately 7 Remove the old battery and insert the new battery 2 Battery type 1 5V AA When inserting the battery pay attention to the L polarity 8 Close the battery compartment Make sure the plug contacts are in the correct position 74 6 3 3 Configuration of transmitter ID and data transmission frequency FRITSCH A The measuring transmission unit 12 is equipped with four configura tion switches for setting the transmitter ID and data transmission fre quency The switches illustrated are all OFF actuator cams set to OFF 6 3 3 1 Adjustment options of the transmitter detection Upon delivery all switches are set OFF This means as identification that it is cup 1 and the transmission frequency is 1 second ID Switch 1 Switch 2 Transmitter no 1 OFF OFF Transmitter no 2 ON OFF Transmitter no 3 OFF ON Transmitter no 4 ON ON NOTICE For the operation of two or more EASY GTM systems each transmitter must have a separate ID 102 FRITSCH A 6 3 3 2 Transmission frequency setting options Transmission every Switch 3 Switch 4 1 second OFF OF
34. d and closed by a motor and therefore not without a connection to the power supply See amp Protection against restart on page 17 E It can only be opened when the mill comes to a stop m The grinding chamber cover must always be closed during grinding E When the grinding chamber cover is open the mill s mechanical unit is locked mechanically to prevent it from starting le FRITSCH A 1 8 Hazardous points 1 9 Electrical safety 1 9 1 General information Crushing hazard when opening and closing the grinding chamber cover the closing force can be adjusted consult Fritsch GmbH Crushing hazard when adjusting the control display Crushing hazard when using the locking lever CAUTION Fire hazard at the grinding bowl after grinding and during the grinding pauses See amp Impact of the ball size and the material during grinding on page 35 The effect of high temperature on page 39 and Cooling the grinding bowl on page 59 DANGER The grinding bowl may open extremely suddenly if the internal pressure is too high Never use brute force to open the bowl Do not fail to observe The effect of high tem perature on page 39 and Safety measures against an excessively high pressure on page 40 The main switch separates the device from the power supply with two poles Turn off the main switch if the planetary micro mill is out of service for prolonge
35. d periods e g overnight J FRITSCH A 1 9 2 Protection against restart In the case of a power failure during operation or after turning the device off at the main switch the grinding chamber cover is locked When the power supply is restored the grinding chamber is not opened until the software detects that the drive is stationary For safety reasons however the planetary micro mill does not restart 1 9 3 Overload protection E Inthe event of an overload the device reduces the speed in a con trolled manner This special operating state is indicated on the dis play m The device shuts down if the drive motor becomes too hot EB The device shuts down if the drive is blocked 1 9 4 Imbalance detection The device shuts down if there is excessive imbalance See amp Using the device on page 27 17 FRITSCH A 2 Technical data 2 1 Dimensions 360 mm x 400 mm x 580 mm height x width x depth 2 2 Weight Net approx 44 kg Gross approx 61 kg 2 3 Operating noise The sound level is approx 74 dB A This value fluctuates significantly depending on the speed and material to be ground and on the type of grinding bowl and grinding balls The device is rated with IP 20 2 4 Voltage The device can be operated in two voltage ranges m Wide range input 100 240 V 10 Transient overvoltage according to overvoltage category Il permitted C If the device is to be operate
36. d with two different voltages e g 115 Vor 230 V it must be disconnected from the power J supply at least 60 seconds before switching over the voltage 2 5 Current consumption The maximum current consumption is approx 10 A 115 V or 5 A 230 V 2 6 Power consumption The maximum power consumption is approx 1100 W 18 FRITSCH A 2 7 Electrical fuses E Fuses on the back of device 2x10 AT 2 8 Material E Maximum feed amount in the case of hard material approx 5 mm E Maximum feed amount 2 x 35 ml 2 9 Final fineness E Dry grinding up to d g lt 20 um depending on the material m Wet grinding up to d lt 0 1 um depending on the material 19 FRITSCH A 3 Installation 3 1 Transport The device is delivered on a transport pallet with a wooden cover We recommend using a forklift or pallet truck for transporting the packed device DANGER Do not step under the transport pallet during transport WARNING Improper lifting can lead to personal injury or property damage The machine is only to be lifted with suitable equipment and by qualified personnel The guarantee excludes all claims for damage due to improper transport 3 2 Unpacking Open the straps of the packaging Remove the lid from the crate or open the crate upwards Remove the accessory cardboard pieces and additional padding Lift the upper part of the packaging off the transport pallet The device
37. des any costs for transport packaging or travel that accrue in the event the product must be sent to us or in the event that one of our specialist technicians is required to come to your site Any servicing done by persons not authorised by us and any use of parts that are not original FRITSCH accessories and spare parts will void the guar antee The guarantee period will neither extend nor will a new period of guar antee begin in the event that a claim is placed against the guarantee Please provide a detailed description of the type of error or the com plaint If no error description is enclosed we shall interpret the shipment as an assignment to remedy all recognisable errors or faults including those not covered by the guarantee Errors or faults not covered by the guarantee shall in this case be rectified at cost We recommend reading the operating manual before contacting us or your dealer in order to avoid unnecessary inconvenience Ownership of defective parts is transferred to us with the delivery of the replacement part the defective part shall be returned to us at buyer s expense NOTICE Please note that in the event that the device must be returned the device must be shipped in the original Fritsch packaging Fritsch GmbH denies all liability for any damage due to improper packaging packaging not from Fritsch Any enquiries must include a reference to the serial number imprinted on the type plate 108
38. ding grinding in a suspension sss22200 38 5 8 1 The effect of high temperature cccccseeccceseeeeeeeeeeees 39 5 8 2 Safety measures against an excessively high pressure 40 5 9 Handling the grinding DOWL cccccessccceseceeesseceeeeeeeeneeees 41 59 1 Dessen 41 5 9 2 Opening the grinding bowl after a grinding operation 41 5 9 3 Closing the grinding DOWL c cccecccccssececesseeeeeeeeeeeenees 42 5 9 4 Inserting the grinding bowl in the grinding bowl holder 44 5 9 5 Removing the grinding DOWL cc csscccsseeeecesseeeeeeeeees 46 5 10 Mass balance enneisa eanaseaeneants 48 5 11 Grinding duration a asneee en 48 5 12 Conducting a grinding Operation ccccecccsseeceseeeseeeees 49 5 12 1 Program sequence after switching ON cccseeeeeeees 50 5 12 2 Starting grinding at high speed ccceeccceeeeeeseeeeeeees 52 5123 Overload een iamesinatoe E EEA 53 5 12 4 Program menu It M ccccccccssssecccsssececeeseeceeeeeeeeeees 53 5 12 5 Saving the current data cccccccssssccccssssccecsesseeesseeeeeeees 54 5 126 L a ding TNE DIOR AI niscscsiarccccaasancaccwnvussanoarsencacsoroaesonenesed 55 5 12 7 Setting the time CONtrOl cccccccsseccccseseceeesseeeceeseeees 56 5 122 Imbalance check nee een een 57 5 12 9 Switching Oft 58 5 12 10 Cooling the grinding DOWL cccccccssseceseseeeeseseeees 59 PRCCOSS ON CS ee er eee
39. e the maximum speed is reduced A reduced speed is indicated briefly by a flashing target speed indicator The Stop button stops the grinding process Press the Info button to display some system information and the type of grinding elements Reference values for the speed limit Ball diameter mm Speeds rpm for Speeds rpm for all agate other materials lt 5 1100 1100 5 900 100 10 750 850 gt 10 600 700 If the planetary micro mill is overloaded the speed is reduced The reduced speed flashes on the display Grinding cycles can be programmed saved and selected here 53 FRITSCH u 1 Press the Menu button in the main menu 2 Then press the Program button gt A new window appears 3 The Current column shows the current parameters of previous entries 0400 n s i ten 4 The Program column shows the data previously stored under DD button 1 00 01 Load 5 12 5 Saving the current data iliyi ET 1 First select the program section that is free or to be overwritten 1100 0000 54 FRITSCH m 2 Then press the Save button to save the current parameters to the selected program section 3 After saving them successfully the new parameters are now dis played in the Program column 5 12 6 Loading the program 1 Select one of the programs 1 8 the various parameter records are displayed in the Program column EB 2
40. e is avail able in the corresponding software manual 93 FRITSCH u 7 General and optional settings 7 1 Standard Operation Procedure It is possible to protect this device by applying SOP mode If this mode is activated by the administrator only stored programs can be loaded for operation Parameters can no longer be changed Some parts of the menu structure can no longer be selected a a 94 7 1 1 Activating SOP mode FRITSCH A 1 Enter a number between 1 and 9999 2 Then Save it 3 Press the lt button to return to the main menu SOP mode is displayed in the main menu 7 1 2 Deactivating SOP mode To disable the restrictions for changing parameters enter the pin code and press the ENTER button Press the lt button to return to the main menu If the device is switched off SOP mode is active again 95 7 1 3 Deleting SOP mode FRITSCH A 1 Deactivate the mode Deactivating SOP mode on page 95 2 Enter pin code 0000 and Save it 3 Press the lt button to return to the main menu 096 FRITSCH zu 7 2 RFID If the bowl is damaged the bowl detection can be deactivated Because the RFID detection is a safety system that cannot simply be deactivated it is protected by a pin code This pin code can only be obtained by consulting Fritsch GmbH 97 FR
41. e limit 6 Press the lt button to confirm your entry and return to the EASY GTM sub menu 81 FRITSCH u 6 3 8 Entering the pressure limit 1 Select the maximum pressure input C If the max pressure is reached the device stops the grinding process and goes into cooling mode L Depending on the setting of the operating mode see amp Selecting the operating mode on page 83 the device stops the grinding process and opens the grinding chamber cover or reduces the speed gradu ally until a minimum speed is reached in order to ach ieve an optimal reduction of pressure 2 Enterthe required max pressure limit DANGER Do not exceed a maximum pressure of 14 bar Otherwise the EASY GTM system and the machine will be damaged 3 Mit lt Taste die Eingabe best tigen und zum Untermen EASY GTM zur ckkehren 4 Select the minimum pressure input 5 Enter the required min pressure limit When the selected min pressure e g 2 bar is reached again during the cooling phase the mill starts the grinding process again 6 Press the lt button to confirm your entry and return to the EASY GTM sub menu 82 FRITSCH mm 6 3 9 Selecting the operating mode You can use the Function menu item to select how the P 7 premium line is to respond to the temperature or pressure limit being reached rpm With this setting the P 7 premium
42. e previous one is deleted or press the C button to delete the current parameter Maximum possible entries are Speed 1100 rpm time 999 min pause 99 min cycles 99 12 After entering the parameters press the lt button to return to the main menu i Ta Press the Start button gt the grinding chamber is closed and the Speed 0400 Pause win OOT safety check starts Cycles 01401 OR 010 Revers off 251 FRITSCH u 14 Various sensors check the bowls and the closing mechanism of the device That will take a few moments The Stop button stops the process Shutter closed v Cup locked X T Type X 15 If the check is successful this is confirmed and grinding is then started without delay 16 If the sensors detect insufficient safety the starting procedure is interrupted and the cause is displayed Press the gt button to open the grinding chamber and move grinding station 1 into the loading position When the error is corrected grinding can be continued Shutter closed v Cup locked X F 5 12 2 Starting grinding at high speed If the speed exceeds 600 rpm the correct ball size must be selected CAUTION If the wrong balls are selected they will be destroyed by the high grinding energy 25 FRITSCH u Select ball diameter Program menu item Depending on the choice of the ball siz
43. ed down any fur ther 7 _ The loading position can only be changed if the locking elements 11 and clamping brackets 10 that are not in their initial posi tions and block the milling mechanism reach their initial positions again correctly NOTICE After a few minutes of grinding and during the cooling phases check that the condition of the grinding bowls is OK see amp Wet grinding grinding in a suspension on page 38 Handling the grinding bowl on page 41 and Inserting the grinding bowl in the grinding bowl holder on page 44 47 FRITSCH zu 5 10 Mass balance Planetary ball mills are generally subject to a specific imbalance during operation To keep this imbalance as low as possible all rotating masses in the system must be balanced as completely as possible To ensure optimum mass balancing imbalance correction of the device identical grinding bowls and identical grinding bowl fillings must always be used at both grinding stations It is quite possible to operate the device with different loads e g dif ferent grinding bowl fillings however that will result in a power loss or depending on the degree of imbalance in the device shutting down The request Please check the imbalance appears on the display See amp Imbalance check on page 57 l NOTICE It is not possible to specify a permitted mass difference and the resulting imbalance exactly The
44. eleration result in high mechanical stress gt impact effect The higher the density of the material to be ground the l higher the mechanical stress is The highest mechanical stress is achieved with balls made of tungsten carbide with a diameter of 20mm If large agate balls are used they could destroy themselves and the grinding bowls That is also the case with sintered corundum and silicon nitride balls Balls with a diameter of 5 mm and less result in high thermal system stress me n FRITSCH A The large surface of many small balls results in high thermal stress due to the friction effect It can already be measured after 5 minutes of grinding above 100 C by a surface sensor on the surface of the lid Inside the grinding bowl the temperature is then much higher an L The adhesive used is permanently resistant to temperatures of up to 140 C If the external temperature does not exceed 100 C the adhesive will hold 5 4 Filling quantities of grinding bowls Grinding bowl Min sample quantity Max sample quantity 20 ml 1 ml 9 ml 45 ml 3 ml 20 ml 80 ml 10 ml 30 ml CAUTION A For wet grinding with large balls with a diameter of gt 10mm at least half the maximum sample quantity must be inserted If the suspension is highly fluid the balls will not have any resistance and the balls and the grinding bowl could be damaged The result is the same as if no material to be ground were filled
45. ely and may even damage it High loads may be heavy loads high speeds high temperatures long oper ating times or combinations of these NOTICE The grinding duration in the reversing mode must not exceed 5 minutes A longer grinding duration in the reversing mode may damage the PULVERISETTE 7 premium line NOTICE If the permissible maximum temperature in the bowl is exceeded during grinding then the device must not be switched off with the lid closed That could lead to heat accumulation in the machine which could cause damage to the device Provide sufficient cooling by letting the mill continue to run at a speed of 100 rpm for approx 20 30 min or by shut ting off the mill with the lid open 5 1 1 General information The grinding bowls have been tested and approved for a static internal pressure of up to 20 bar If the pressure increases gradually safety elements in the lid prevent the build up of an unacceptable overpressure Fast and dynamic pressure surges e g an explosion or very fast chemical reactions etc up to 30 bar will not cause any damage A higher pres sure will result in irreparable damage to the grinding bowl and possibly also damage the machine In such a case the grinding bowls and the machine are not covered by the Fritsch guarantee To clean the grinding bowl and its components follow the operating instructions precisely amp Cleaning on page 104 28 FRITSC
46. er 11 of the connection on the hose inwards 11 Locking lever 2 Push the hose connection onto the valve 8 and down onto the inner seal At the same time the valve is opened by an internal pin in the hose connection When the locking lever is released it engages on the valve thread 63 FRITSCH A 3 For flushing the second valve can be opened with a pen e g the tip of a ballpoint pen NOTICE The gas must be supplied very slowly to avoid any turbu lence in the grinding bowl or of the material to be ground when it is inserted 4 After gassing the sample remove the hose 7 again The grinding bowls are inserted and handled as shown in amp Using the device on page 27 6 1 4 Removing the gassing lid in individual steps 1 Turn the central handle 9 and remove it by hand 8 Valve 9 Gassing lid handle 10 Actuating pin 64 FRITSCH A 10 Actuating pin 2 Unscrew the two actuating pins 10 with a broad slotted screw driver tightening torque approx 4 5Nm maximum manual force 3 Unscrew the two valves 8 using the socket wrench 1 tightening torque approx 3 5 4Nm maximum manual force 4 Remove the flat seals 4 under the valves The flat seals are deformed by the contact pressure 4 Flat seal wien FRITSCH A 5 Valve insert 5 Turn the two valve inserts out of the valves using
47. er card entitled Securing of Guarantee enclosed with the device must be properly filled out and despatched without delay after receipt of the device and be received by us within three weeks or alternatively online registration must be carried out with the above mentioned information The guarantee will not be granted in cases where E Damage has arisen due to normal wear and tear especially for wear parts such as Crushing jaws support walls grinding bowls grinding balls sieve plates brush strips grinding sets grinding disks rotors sieve rings pin inserts conversion kits sieve inserts bottom sieves grinding inserts cutting tools sieve cassettes sieve and measuring cell glasses E Repairs adaptations or modifications were made to the device by unauthorized persons or companies E The device was not used in a laboratory environment and or has been used in continuous operation E Damage is present due to external factors lightning water fire or similar or improper handling E Damage is present that only insubstantially affects the value or proper functioning of the device m The device type or serial number on the device has been changed deleted removed or in any other way rendered illegible E The above mentioned documents have been changed in any way or rendered illegible 107 FRITSCH A Costs not covered by the guarantee Further information about the guar antee This guarantee exclu
48. exposed to thermal shocks as this could cause irreparable damage to the parts gt They will fall apart in an explosive manner 8 2 Mill DANGER Mains voltage Before beginning with cleaning work disconnect the mains plug and protect the device against being unin tentionally switched back on Do not allow any liquids to flow into the device Indicate cleaning work with warning signs Put safety equipment back into operation after cleaning work The micro mill can be wiped down with a damp cloth when it is switched off The grinding chamber can be cleaned thoroughly with a damp cloth by removing the grinding chamber cover 104 FRITSCH A 8 2 1 Removing the grinding chamber cover 1 Remove the 4 screws from the side of the housing using a screw driver 2 Then carefully tilt the grinding chamber cover to the right 4 After doing this the cover can be lifted off completely and the grinding chamber can be cleaned 5 Tofitthe grinding chamber cover proceed in the reverse order DANGER Do not allow any liquids to flow into the device 105 FRITSCH A 9 Maintenance DANGER Mains voltage Maintenance work may only be performed by special ised personnel Before beginning with maintenance work unplug the mains plug and protect the device against being unin tentionally switched back on Put safety equipment back i
49. f the completely filled grinding bowl 12 5 g 3 The spring must be pressed to be able to insert the washers 91 FRITSCH A 4 Make sure that the green rubber washer 2 is lying at the top 5 Now turn the lock nut 1 onto the threaded spindle To do this push the spring back 6 Turn the lock nut 1 by hand until it touches the rubber washer 2 7 _ Now insert the 2 hole face wrench 5 in the 2 holes of the bowl 8 Tighten the lock nut 1 very firmly using the pipe wrench 6 CAUTION Check after the first 5 minutes of grinding if the lock nut has been released If that is the case it must be firmly re tight ened 92 FRITSCH A 6 6 Planetary mills MillControl software The PULVERISETTE 7 premium line planetary mill is con trolled either at the device using the clearly arranged touch display or with the MillControl software The software pro vides the user with all device controlling options and adds further aspects to the operation of the planetary ball mills like the conduction of identical grinding cycles but also grinding operations using the SOPs In addition you also have the option of having your grinding operations evalu ated in detail in standardised reports with the relevant parameters If an EASY GTM system is used all important data of this system can be displayed in the program Detailed information on the MillControl softwar
50. g the GeVICE ccccccccesseccceseccccesececeeseceeeueceeeeneceeseseeesees 27 5 1 Saey MM OMe Cl on ee 27 5 1 1 General information 22002420008enne nenne nnennn nennen 28 5 1 2 Overpressure relief of the grinding bow s 29 FRITSCH A 5 1 3 Grinding bowl lid eeccccssseccceeseeceeeeeceesseeseeeseeeeeees 31 5 2 Choice of grinding bowls and grinding balls 31 5 2 1 Useful capacity of the grinding bow s u 33 5 2 2 Size of the grinding balls ceecccssscceeesseceeseeeeeeeeeees 33 5 2 3 Number of balls per grinding bowl independent of the material QUANTITY sncuascaccosrarancaasanssanennstsednaenataeacnanecaesacnsts 34 5 2 4 Calculated weight of a ball ecccccescecesseeeeeeeeeeneeees 35 5 3 Impact of the ball size and the material during grinding 35 5 4 Filling quantities of grinding DOWIS cccsssecceseeeeeeeeees 36 5 5 Filling the grinding DOWL ccsccccssscceesececeseeeeeeeeeeeeeeens 37 5 6 Factors with an impact on Srinding cccscccssesceeseeeeeeees 37 5 6 1 Running time grinding duration ccccccseeseeeeseeeeees 37 5302 SS EO ia nee ea nee ra nee 37 5 03 Reverse MOORE ann 37 5 6 4 Number and size of the balls 0s2220022200 Bene eeeenn 38 5 6 5 Weight of the balls type of material 38 5 7 DENA ee er 38 5 8 Wet grin
51. gassing lid fitting 2 Unscrew the two actuating pins 7 with a broad slotted screw driver tightening torque approx 4 5Nm maximum manual force 7 Actuating pin 70 FRITSCH A 3 Unscrew the two valves 3 and 4 using the size 11 single head wrench 11 tightening torque approx 3 5 4Nm maximum manual force 4 Gassing valve quick release coupling 5 Sealing ring 8x12x1mm vulcanised fibre 6 Flat seal 8 Gassing lid insert 4 Remove the seals 5 and 6 from under the valves The seals are deformed by the contact pressure NOTICE Do not forget to insert the two valve flat seals 5 and 6 5 The gassing lid is fitted in the reverse order 3 Gassing valve connecting plug 5 Sealing ring 8x12x1mm vulcanised fibre 6 Flat seal 8 Gassing lid insert 6 3 EASY GTM Gas Pressure and Temperature Measuring System The EASY GTM gas pressure and temperature measuring system is used to control the grinding process and for mechanical alloying NOTICE If grinding balls with a diameter of 1 mm are used there is a risk of the clearance holes of the lid getting clogged which could falsify the pressure and temperature measure ment Grinding balls with a diameter of up to 0 8 mm or grinding balls with a diameter of 1 2 mm or greater can be used without any problem 71 FRITSCH A 6 3 1 Case contents and system design e un 1 2 6 Nm torque spanner hexagonal
52. he grinding chamber cover 105 IVT ANTE NAICS see een 106 Guarantee terms een 107 Exclusion of liability cccccccccccsscccssecceseceeeeceeeeceseeeeeeees 109 Safety lOgbOOK ccccccssecceseecceseceeseceeesceeeneceeusceseeceeeneees 111 INDEX 113 _ FRITSCH 1 Safety information and use 1 1 Requirements for the user 1 2 Scope of application This operating manual is intended for persons assigned with operating and monitoring the Fritsch PULVERISETTE 7 premium line The operating manual and especially its safety instructions are to be observed by all persons working on or with this device In addition the applicable rules and regulations for accident prevention at the installation site are to be observed Always keep the operating manual at the installation site of the PULVERISETTE 7 premium line People with health problems or under the influence of medication drugs alcohol or exhaustion must not operate this device The PULVERISETTE 7 premium line may only be operated by authorised persons and serviced or repaired by trained specialists All commis sioning maintenance and repair work may only be carried out by techni cally qualified personnel Qualified personnel are persons who because of their education experience and training as well as their knowledge of relevant standards regulations accident prevention guidelines and oper ating conditions are authorised
53. her obligation is explicit or implicit contractual or arising from unlawful acts or prescribed contractually by law or otherwise In no event shall the buyer be entitled to any compensation from Fritsch GmbH for any special direct indirect coincidental or consequential damage including but not limited to lost profits lost savings lost sales or financial loss of any kind or for compensation of third parties for downtimes for lost goodwill for damage to or replacement of equip ment and property for costs or restoration of materials or goods related to the product or the use of our products for other damage or injury to persons including fatal injuries or similar The above exclusion of lia bility is limited by mandatory liability as prescribed by laws or jurispru dence Liability for negligence is excluded in all cases No permission is given expressly implicitly or otherwise for the use of patents brands or other copyrights We also assume no liability for copy right infringements or infringements of the rights of third parties arising from the use of this product Neither compliance with this operating manual nor the conditions and methods used during installation operation use and maintenance of the product can be monitored by Fritsch GmbH Improper execution of the installation can result in property damage and thus endanger persons Therefore we assume absolutely no responsibility or liability for loss damage or costs that
54. ing manual is always near the device The PULVERISETTE 7 premium line may exclusively be used within the scope of applications set down in this manual and within the framework of guidelines put forth in this manual In case of non compliance or improper use the customer assumes full liability for the functional capa bility of the PULVERISETTE 7 and for any damage or injury arising from failure to fulfil this obligation By using the PULVERISETTE 7 premium line the customer agrees with this and recognizes that defects malfunctions or errors cannot be completely excluded To prevent risk of damage to persons or property or of other direct or indirect damage resulting from this or other causes the cus tomer must implement sufficient and comprehensive safety measures for working with the PULVERISETTE 7 premium line aw I EEE ae 7 a 7 Neither compliance with this manual nor the conditions and methods used during installation operation use and maintenance of the PUL VERISETTE 7 premium line can be monitored by Fritsch GmbH Improper execution of the installation can result in property damage and thus endanger persons Therefore we assume absolutely no responsibility or liability for loss damage or costs that result from errors at installation improper operation or improper use or improper maintenance or are in any way connected to these The applicable accident prevention guidelines must be complied with
55. ins 7 on the flat seal 9 in the bowl 3 Hold the lid 2 at the hooks Push the hooks outwards and place the lid 2 on the bowl above the gassing lid insert 8 4 The central handle 1 must be removed as illustrated 5 Turn the lid 2 with the hooks pressed outwards on the bowl until the lugs of the hooks engage in the recesses on the edge of the bowl fitting amp Closing the grinding bowl on page 42 After releasing the hooks they must be immersed completely in the recesses on the outer diameter of the bowl fitting and be exactly vertical 68 6 Push the central handle 1 down by hand until the resistance increases Use the hexagon socket wrench 10 to tighten it with maximum manual force The maximum manual force is equivalent to atorque of approx 3 5 4Nm FRITSCH A 7 This is what the closed grinding bowl looks like a Quick release coupling structure with screwed pipe fitting b Quick release coupling connector with screwed pipe fitting 69 FRITSCH A These parts are not included in the scope of delivery They are only one example of how gassing hoses can be connected to the hose couplings Fixed 2 8 mm polyamide hoses are connected here by a threaded hose connection 6 2 4 Removing the gassing lid in individual steps 1 Turn the central handle 1 and remove it by hand 1 Compl gassing lid handle 2 Compl
56. it breakers which are adapted for operation with frequency converters are commercially available Operation without a residual current switch is possible but must be done in accordance with the relevant regulations I 4 Initial start up FRITSCH A Switch on the device only after all work as described in amp Installation on page 20 has been carried out 4 1 Switching on 1 Connect the device to the power supply using the cable provided device cable with IEC 320 C13 plug sulverisette 7 a 2 Ger t am Hauptschalter einschalten 3 The display lights up 4 2 Function check Grinding station 1 is moved into the loading position The grinding chamber cover opens Check if grinding station 1 is empty no bowl inserted Press BUTTON 2 on the display Cup Position _ je Grinding station 2 is moved into the loading position pee Check if grinding station 2 is empty Press the lt button for confirmation and to access the main menu Heed 1100 00 Cycles O1 OI T p j ress the Menu button Time O05 Revers Off E VL i Open Start Stop 24 9 You can make various settings in the next menu Select the Parameters menu item FRITSCH A es 10 A sub menu appears in which you can enter the speed using the lt gt 0400 n input keys Set the speed to 100 DODD wis 11 Press the lt
57. ive samples Medium hard brittle samples Hard brittle samples Hard abrasive sam ples The grinding bowls and grinding balls made of zirconium oxide are resistant to acids apart from hydrofluoric acid Normally choose a grinding bowl and grinding balls that are made of the same material Tey FRITSCH A Exception Tungsten carbide balls lt 20 mm may be temporarily a few minutes combined with grinding bowls made of tempered steel 5 2 1 Useful capacity of the grinding bowls Grinding bowl 20 ml 45 ml 80 ml Useful capacity 1 9 ml 3 20 ml 10 30 ml material to be ground 5 2 2 Size of the grinding balls Type of feed material Hard samples with a maximum feed size of 5mm Average feed size of 0 5 1 mm Fine material 0 1 0 5 mm Very fine material lt 0 1 mm Homogenisation of dry or liquid samples Suitable ball diameter 15 mm 20 mm 15 mm 10 mm 10 mm 5 mm 3 mm and smaller 10 mm 5 mm NOTICE It is not advisable to mix balls of different diameters If balls with different diameters are used increased wear to the balls is to be expected 33 FRITSCH A 5 2 3 Number of balls per grinding bowl independent of the material quantity A higher number of balls will reduce the grinding duration and the grinding results will be within a smaller grain size range The number of balls should be complied with to avoid unnecessary wear Ball diameter mm Grinding bowl
58. l pressure has been released completely Observe the opening instructions in amp Opening the grinding bowl after a grinding operation on page 41 and Safety measures against an excessively high pressure on page 40 The device may only be operated indoors The sur rounding air must not contain any electrically conduc tive dust When grinding oxidisable substances e g metal or coal there is a risk of soontaneous combustion dust explosion if the proportion of fine particles exceeds a certain percentage Chemical reactions are also pos sible during wet grinding When grinding these kinds of substances special safety measures e g wet grinding must be taken and the work must be supervised by a specialist The device is not explosion protected and is not suit able for grinding explosive materials DANGER Do not reuse damaged accessories If the planetary micro mill or its components are dam aged or if its operation is not as described in the oper ating manual the device may not be put into service In such a case consult your Fritsch GmbH representative or distributor WARNING The maximum accepted concentration MAC levels of the valid safety regulations must be observed If necessary ventilation must be provided or the machine must be oper ated under an extractor hood 14 FRITSCH CAUTION Wear hearing protection Above a sound level of 90dB A Wea
59. ments for the user 0 00000 8 Reversing Mode 00 ee eee eee 37 S Safety information 0 0 0 eee ee eee 10 Safety information for using the device 27 Safety logbook 2 0002s 111 112 Safety measures against an excessively high pres SUC a Gee eee aka ea ee ee ea eo ye are 40 Saving the current data 000 ee 54 Scope of delivery 0 meer 60 Screen brightness 0 0 0 0 cece eee eee 99 Selecting the grinding balls 31 Selecting the grinding bowl 31 Selecting the operating mode for EasyGTM 83 SOD au Oo ee ee oe ee ea 21 Setting the time control 2 222222 56 Size of the grinding balls 0 33 Skilled workers 2 222222 seen 8 Special emptying device for grinding bowls 86 SPCC oes oes ba oe ee eee ee 37 Standard gassinglid 2 0 0 60 Standard Operation Procedure 94 Starting grinding at high speed 52 Switching Off 0 2 0 ee ee 26 58 Switching ON aaa 24 System information 0 000 eee eee 100 T Transmission frequency setting options 76 U NPSEKIND 56s 8 2 0 00 Hawk Boo Oe ee oe ee at 20 Useful capacity of the grinding bowls 33 V MOSE oct oo acne ace od ow oe bare Be ase 18 W Warning information 2222er 10 VID ee Hk Oh Bhs ee a 18 Weight ofaball 0 0 eee eee 35 Wet grinding 0 0
60. ns voltage The device may only be operated indoors The surrounding air may not carry any electrically con ductive dust Maximum relative humidity 80 for temperatures up to 31 C linearly decreasing down to 50 relative humidity at 40 C m The room temperature has to stay between 5 40 C m Altitudes up to 2000 m BE Degree of pollution 2 according to IEC 664 3 5 Electrical connection DANGER Provide short circuit protection Risk of damage due to short circuits Make sure that the socket is connected to a mains line protected with a residual current circuit breaker Before establishing the connection compare the voltage and current values stated on the type plate with the values of the power supply system to be used DANGER Mains voltage Changes to the connection line may only be made by a qualified person CAUTION Ignoring the values on the type plate may result in damage to the electrical and mechanical components 22 FRITSCH mm NOTICE Fritsch mills are speed controlled The devices are equipped for this with frequency converters In order to comply with the EMC directive many measures must be taken to pre vent operational transient emissions The possible leakage currents resulting from filtering meas ures can trigger a conventional residual current circuit breaker in the mains line This is no defect To prevent this special residual current circu
61. nto operation after mainte nance work Indicate maintenance work with warning signs We recommend keeping a safety logbook Chapter 12 Safety logbook on page 111 where all work maintenance repairs performed on the device is entered C The most important element of maintenance is regular L cleaning 106 _ FRITSCH 10 Guarantee terms Guarantee period Conditions for claims against the guar antee Reasons for loss of the guarantee As manufacturer FRITSCH GmbH provides above and beyond any guar antee claims against the seller a guaranty valid for the duration of two years from the date of issue of the guarantee certificate supplied with the device Within this guarantee period we shall remedy all deficiencies due to material or manufacturing defects free of charge Rectification may take the form of either repair or replacement of the device at our sole discre tion The guarantee may be redeemed in all countries in which this FRITSCH device is sold with our authorisation This guarantee is subject to the condition that the device is operated according to the instructions for use operating manual and its intended use Claims against the guarantee must include presentation of the original receipt stating the date of purchase and name of the dealer together with the complete device type and serial number For this guarantee to take effect the answ
62. parts to be able to clean the seals properly as well Then dry the parts with a cloth ora blow dryer During installation pay attention to the correct sequence and position of the seals see amp Design on page 87 Funnel lid for special emptying device Flat seal 58x41x2 0 Stainless steel strainer Flat seal 50 5x41x1 5 Adapter for special emptying device O ring 49x4 NOW BW DN The device is generally subject to a specific imbalance during operation To keep this imbalance as low as possible all rotating masses in the system must be balanced as completely as possible To ensure optimum mass balancing imbalance correction of the device identical weights must always be used at both grinding stations amp Mass balance on page 48 The counterweight is used for weight balancing if only one grinding bowl is inserted with a sample in the p 7 premium line 90 6 5 1 Design FRITSCH A Lock nut Rubber washer Counterweights 25 g each Bowl counterweight AUNE 6 5 2 Handling Lock nut Rubber washer Compensating washers 25 g each Counterweight 2 hole face wrench Pipe wrench NUM PwmN FR 1 Determine the weight of the grinding bowl to be used with lid material to be ground and balls 2 Then weigh the counterweight 4 and fit compensating washers 3 until the complete weight with rubber washer 2 and lock nut 1 of the complete counterweight matches the weight o
63. pressure of up to 40 bar Because the overpressure relief does not work in the case of sudden pressure surges we would like to warn you explicitly that in the event of an explosion in the grinding bowl the hooks could be torn off DANGER Danger to life An explosion in the grinding bowl may cause severe injuries and damage to the device In the context of our product monitoring we would like to inform you about the following damage cases that have occurred E During dry grinding of a light alloy resin mixture there was a severe explosion of the grinding bowl after 64 cycles 5 min grinding 10 min pause 800 rpm that completely destroyed the device E During wet grinding of silicone powder in DEGBE solvent there was an explosion in the grinding bowl exploded after 11 cycles 10 min grinding 30 min pause that ripped off the locking hooks of the grinding bowl lid The grinding bowl lid caused irreparable damage to the mill hood and the safety blocking mechanism stopped the mill E During dry grinding of a silicon compound in grinding conditions not known to us and not disclosed by the customer there was an explo sion of the grinding bowl that ripped the locking hooks off the grinding bowl lid 5 2 Choice of grinding bowls and grinding balls CAUTION If the grinding elements used are not genuine accessories we assume no guarantee and exclude all liability for damage to the device or for personal injury
64. r safety gloves The grinding bowls may get very hot See Hazardous points on page 16 The effect of high temperature on page 39 and Cooling the grinding bowl on page 59 Do not grind with the device for several hours in suc cession without cooling phases Risk of overheating The device may not be run without supervision In cer tain operating states the vibrations may result in a shifting effect on the surface E Do not remove the information signs E Unauthorised alteration of the device will void Fritsch s declaration of conformity to European directives and void the guarantee m If after reading the operating manual there are still questions or problems please do not hesitate to contact our specialists 1 7 Protective equipment 6 Protective equipment is to be used as intended and may not be disabled or removed All protective equipment is to be regularly checked for integrity and proper functioning DANGER The valves on the grinding bowls may not be repaired Each time before using the planetary micro mill check that the pro tective equipment is not damaged or contaminated see Haz ardous points on page 16 Electrical safety on page 16 and Safety information on page 27 E Do not make any changes to the protective equipment apart from the maintenance tasks listed in the operating manual m The device s grinding chamber cover can only be opene
65. resulting from a reaction of the sample material in the grinding bowl that cannot be anticipated or controlled Bear in mind that it is essential that test grinding operations with unknown parameters are always carried out in a safe room that reliably prevents damage by exploding grinding elements WARNING Make sure before starting the machine that the grinding bowls have been tensioned correctly and that there are no loose parts inside the device There is a risk of loose grinding bowls or parts being flung out Failure to observe this will void the guarantee and release us from liability for any resulting damage to the device or personal injury NOTICE During grinding the temperatures in the grinding bowl may get very high In encased grinding bowls the inserts are glued into the casing with a two component construction adhesive The adhesive is resistant to temperatures up to approx 140 C Above 140 C the adhesive will liquefy and accumulate below the insert in the casing When the adhesive cools down it solidifies and pushes the casing up That can cause irreparable damage to the insert The grinding bowl will definitely be rendered unusable Above temperatures of 200 C the adhesive will be destroyed The same applies for encased grinding bowl lids 27 FRITSCH A NOTICE The planetary drive is provided by the main disc via a toothed belt drive Constant high loads stress the toothed belt sever
66. rews are secured against becoming loose during the grinding process once they have been tightened with the torque spanner as described Fritsch GmbH assumes no guarantee for damage p caused by grinding with loose screws 77 FRITSCH A 5 Switch on the transmitter with the On Off button A and insert the bowl as described in 6 Inserting the grinding bowl in the grinding bowl holder on page 44 NOTICE Check the fitting of the transmission unit again after inserting the bowl NOTICE During a grinding during the pauses the correct position of the Allen screws of the transmission unit must to be checked If screws became loose re tighten them 6 3 5 Installation of the receiver board in the P 7 premium line DANGER Before starting the installation disconnect the mains plug and protect the device against being unintentionally switched back on Secure installation work with a warning sign 1 The 6 screws e used to attach the rear panel to the housing are undone and the rear panel is opened carefully 78 FRITSCH A 2 The PKM interfaces board 81 0011 00 is on the rear panel with the slot f for the receiver module 81 0013 00 3 Insert the receiver module in the corresponding slot As illus trated 4 Close the rear panel of the housing again and screw it tight 6 3 6 Activating EASY GTM If the device is protected by SOP mode
67. rute force to open the bowl AQ FRITSCH A 5 9 Handling the grinding bowl 5 9 1 Design Compl bowl Compl lid Flat seal Locking hook Compl handle Valve plug Press on sleeve Actuating pin Lid insert WO COON DU BWN PE 5 9 2 Opening the grinding bowl after a grinding operation 1 Allow the bowl 1 to cool down 2 Release the pressure by turning the press on sleeve 7 to open it l NOTICE After releasing the pressure via the press on sleeve this and the valve plugs 6 must be cleaned thor oughly before further grinding processes If this is not done the tightness may be reduced due to residual sample material After restarting and reaching the set speed we rec ommend securing the press on sleeve 7 and handle 5 again 3 Turn the handle 5 to open it 41 FRITSCH A 4 Ifthe lid insert 9 is sticking on the flat seal 3 apply a screw driver to the actuating pin 8 to remove the lid insert 9 from the flat seal 3 5 Open the lid 2 5 9 3 Closing the grinding bowl 1 Insert the flat seal 3 in such a way that the recess is near a locking hook 4 Attention 2 Push the locking hooks 4 inwards completely at the top end and place the lid 2 on the bowl 1 42 3 The lid 2 is now lying on the small lug a of the locking hook 4 on the edge of the bowl FRITSCH A a Lug
68. rweight 0008 91 Device safety information 0005 13 DIMENSIONS 4 44 54 EEE 18 Dry SUING sa Reese nenne 38 E EASY GIM ierre nenep eraa a e 71 Effect of high temperature 2 22220 39 Electrical connection 2 22 222er 22 Electrical fuses 2 222220 one ee es 19 Electrical safety 2222 comme 16 Entering the pressure limit 004 82 Entering the temperature limit 81 Exclusion oflliability 2 22222220 109 Explanation ofsigns 222 222er 10 Explanation ofsymbols 2 2222 10 F Filling quantities of grinding bowls 36 Filling the grinding bowl 0 37 Finalfineness 0 ee ee ee es 19 Firmware update 2 0 eee ee ees 102 Fitting the gassing lid on the grinding bowl 61 Fitting the gassing lid swagelok 67 TONCHON CHECK es eee ae eee oe eae ee Oe ee 24 G Gassing lid Swagelok 2 00200 eee 66 Scope of delivery 2 0 eee eee ees 67 Grinding bowllid 2 0 00 31 Grinding duration 0 0 0 eee 37 48 Guarantee termS 2 0 0 0 cee ee es 107 H Handling of the counterweight 91 Handling the special emptying device 87 Hazardous points 2 2 2m ee ns 16 Hose adapter for grinding bowl gassing 63 69 I Imbalance check nunnana anaa 57 Imbalance detection ssn anana eee ee ee 17 Impact Or the HallSs 2e 5 r ass sa
69. safe ERITSCH Material bowl and balls Agate Silicon nitride Sintered corundum Zirconium oxide Stainless steel Tempered steel Tungsten carbide A CAUTION The grinding element is subject to normal wear during use Before every grinding operation check the wall thickness of the grinding bowls In the event of severe wear replace the grinding bowl If this is not done the prevailing high centri fugal forces during grinding may cause the grinding balls to penetrate the bowl s wall and damage the mill Failure to observe this will render void the guarantee and release us from liability for any resulting damage to the device or per sonal injury The hardness and density specific weight of the grinding bowl and grinding balls used must be greater than that of the material used to prevent excessive wear by abrasion Main components of the material 99 9 SiO 90 SizN 99 7 Al O3 96 2 ZrO Bowl 17 19 Cr 8 10 Ni Balls 12 5 14 5 Cr 1 Ni Bowl 11 12 Cr Balls 1 0 1 65 Cr 93 WC 6 Co Density in g cm High density means high impact energy 2 65 3 25 3 9 57 7 8 79 14 9 Abrasion resistance Good Extremely good Fairly good Very good Fairly good Good Very good Use for grinding stock Soft to medium hard samples Abrasive samples metal free grinding Medium hard fibrous samples Fibrous abras
70. switch on the device The USB port is now automatically activated Start the PROGRAMMER EXE software and then select the firm ware file for programming VG UL FRITSCH A 5 Select the newly installed COM port here 6 Press Program to start the update A GERATEDOKUMENTATION Programmierung PKM PKM PL P7 V113 det Task Ready mm TD E 102 FRITSCH A 7 After programming Information 8 Now connect the flasher software 9 Switch off the planetary micro mill not the computer for a few seconds 10 Switch the device back on again gt Finished 103 FRITSCH A 8 Cleaning 8 1 Grinding elements Clean the grinding bowl and grinding balls each time after using them e g clean them under running water using a brush and a commercially available cleaning agent Add sand and water until the grinding bowl is about half full and grind to clean for 2 to 3 minutes in the laboratory planetary mill Cleaning with an ultrasonic cleaner is permitted For sterilisation in the heat cabinet only heat the grinding elements up to 120 C Grinding elements made of agate may only be heated up to 100 C CAUTION Cool grinding elements made of agate sintered corundum zirconium oxide and silicon nitride slowly and carefully Do not heat the grinding elements in a microwave under any circumstances heating is too fast They must never be
71. the regional recycling point collection point Please only place dis charged flat batteries in the containers intended for this purpose Cover the terminals of lithium batteries with adhesive tape first All batteries and rechargeable batteries are reused Valuable substances such as zinc iron and nickel can thus be recycled Battery recycling is one of the easiest environmental protection measures The crossed out dustbin symbol means that rechargeable batteries may not be disposed of along with household waste You can of course also return discharged batteries with sufficient postage by post to Fritsch GmbH Milling and Sizing Industriestrasse 8 D 55743 Idar Oberstein Germany For information on removing the battery see Inserting changing the battery on page 72 6 4 Special emptying device for grinding bowls Special emptying device for grinding bowls of PULVERISETTE 7 premium line enables the fast and simple separation of the grinding balls and sus pension after grinding It is suitable for all grinding bowl sizes 80 ml 45 ml and 20 ml 2 strainers with a mesh width of 0 08 mm and 0 8 mm are available 86 FRITSCH A 6 4 1 Design Syringe pump tip Funnel lid for special emptying device Flat seal 58x41x2 0 Stainless steel strainer Flat seal 50 5x41x1 5 Adapter for special emptying device O ring 49x4 NOW BWDN 6 4 2 Handling 1 Remove the bowl with the balls
72. the valve key 6 Tightening torque approx 1 5 2Nm average manual force The valve is held in place using the socket wrench 1 and the valve insert 5 is removed using the valve key 6 NOTICE Do not forget to insert the two valve flat seals 4 6 The gassing lid is removed in the reverse order 4 Flat seal 6 2 Gassing lid with stainless steel swagelok hose couplings NOTICE Our workers perform a water bath test on all gassing lids The part to be tested is sealed a pressure of 5 5 bar is applied and it is immersed in a water bath If there is a leak bubbles will develop The air bubbles that develop within a specific interval are evaluated by the worker tester Only gassing lids with a leak rate of lt 10 mbar I s are approved 66 6 2 1 Scope of delivery lid design FRITSCH A lt Actuating pin Gassing lid insert Flat seal 57 5x48x2 silicone O Hexagon socket wrench size 13 1 Single head wrench size 11 Compl gassing lid handle Compl gassing lid fitting Gassing valve connecting plug Gassing valve quick release coupling Sealing ring 8x12x1mm vulcanised fibre Flat seal av PwmN FR e e O O N 6 2 2 Fitting the gassing lid on the grinding bowl F 1 Place the silicone flat seal 9 on the edge of the bowl insert 267 FRITSCH A 2 Place the gassing lid insert 8 with the seal gassing valves 3 and 4 and actuating p
73. these purposes only FRITSCH u 1 2 1 Operating principle C a Rotation of the grinding bowl b Centrifugal force c Rotation of the support disc Sa Be I Zu The source material is crushed and ground by grinding balls in a grinding u b bowl The centrifugal forces from the rotation of the grinding bowls around their own axis and from the rotating support disc have an effect on the contents of the grinding bowl consisting of material to be ground and grinding balls The grinding bowl and the support disc have opposite directions of rota tion in order that the centrifugal forces alternate in the same direction and in the opposite direction The result is that the grinding balls run down the inside of the bowl s wall with a friction effect and the grinding balls hit the opposite wall of the grinding bowl with an impact effect 1 2 2 Drive motor and speed regulation A maintenance free electric motor operated via frequency converter is used as the drive 1 3 Obligations of the operator Before using the PULVERISETTE 7 premium line this manual is to be carefully read and understood The use of the PULVERISETTE 7 premium line requires technical knowledge only commercial use is permitted The operating personnel must be familiar with the content of the oper ating manual For this reason it is very important that these persons actually receive the present operating manual Ensure that the operat
74. ucting a grinding operation DANGER Explosion hazard Ignition hazard Burn hazard Wear safety goggles Wear safety gloves The following needs to be observed when grinding material for which there is no experience with premium line Initially a grinding duration of 5 minutes should be set and the tempera ture measured on the actuating pin using a surface thermometer If it is below 80 C grinding can be continued until a temperature of 90 C is reached At this temperature it is advisable to apply a cooling pause of about 15 30 minutes At the end of the cooling pause open the knurled screw to check if pressure has built up in the bowl If there is no high pressure the grinding and pause times can be programmed in such a way that the temperature does not exceed 90 C During the pause the mill continues to run at low speed for better cooling From firmware V1 08 and higher If prolonged blow off noises and the discharge of source material sus pension indicate a high internal pressure after cooling take special care when you continue to grind The pressure must always be released after the cooling pauses at least for 30 minutes in order that the suspension can settle to prevent it from getting too high Sooner or later the increase in pressure will stop 49 5 12 1 Program sequence after switching on FRITSCH A 1 Turn the device on at the main switch 2
75. una sense 35 ofthematerial 2222er 35 Mitel Stare sn 6 4 280 0 rennt 24 Inserting changing the battery in the transmission unit of the EGTM 2 ee ee ee ee 72 Inserting the grinding bowl 44 Installation of the receiver board 78 Installation of the transmission unit 76 Intended use 22 ee eee 8 EWC CSc ee re ea Bee a we A 101 L Language setting 2 000 ee ee ee eee 98 Loading the program 00000 e eae 55 M Mass balance ee ee ee es 48 Material seca cae an ee ee Ge ee et ae ee a 19 Menu item POSTAT 246 bch are ee es 53 MillControl Software 2 2 222222 een 93 N Number of balls per grinding bowl 34 FRITSCH A O Opening the grinding bowl 41 Operating noise 1 ee es 18 Operating principle 2 0 2 eee ees 9 ONE OO aa nad en a E eo oo a a es 53 Overload protection 002s 17 Overpressure relief of the grinding bowls 29 p Power consumption 02 02 eee aes 18 Program sequence after switchingon 50 Protection against restart 2 2 2 222 17 Protective equipment 020 ee eee 15 R Removing the gassing lid 2 4 64 Removing the gassing lid swagelok 70 Removing the grinding bowl 46 Removing the grinding chamber cover 105 Replacing the seal 2 2 0 ee ee eee 85 Require
76. ure after the cooling phase otherwise it could be retained in the bowl in spite of cooling That is in particular also the case in the event of a chemical reaction in the grinding bowl See Impact of the ball size and the material during grinding on page 35 Safety measures against an exces sively high pressure on page 40 and Cooling the grinding bowl on page 59 39 FRITSCH A NOTICE If the permissible maximum temperature in the bowl is exceeded during grinding then the device must not be switched off with the lid closed That could lead to heat accumulation in the machine which could cause damage to the device Provide sufficient cooling by letting the mill continue to run at a speed of 100 rpm for approx 20 30 min or by shut ting off the mill with the lid open The bowl may get stuck on the holder if the bowl temperature gets too high In such a case wait until the bowl has cooled down sufficiently in order that it is released by the holder 5 8 2 Safety measures against an excessively high pressure Safety measures against an excessively high pressure 1 Recess To prevent damage to the grinding bowls and the device the flat seal has a small recess on its external diameter The pressure may be released at this point if the insert is lifted by the internal pressure in the bowl That is the case with an internal pressure of about 20 bar Use genuine Seals only WARNING Never use b
77. witched off with the lid closed That could lead to heat accumulation in the machine which could cause damage to the device Provide sufficient cooling by letting the mill continue to run at a speed of 100 rpm for approx 20 30 min or by shut ting off the mill with the lid open 1 Press STOP on the display 2 When the drive comes to a stop grinding station 1 is moved into the loading position and the grinding chamber cover opens auto matically 3 If the device is put out of service for a lengthy period close the grinding chamber cover and turn the device off at the main switch 58 FRITSCH A 5 12 10 Cooling the grinding bowl The grinding bowls can be cooled 1 with the grinding chamber cover open and the fan running the fan continues to run for 1 minute 2 or by the programmed pause times with closed locked grinding chamber cover and the fan running 59 FRITSCH A 6 Accessories 6 1 Standard gassing lid for grinding with inert gas NOTICE Our workers perform a water bath test on all gassing lids The part to be tested is sealed a pressure of 5 5 bar is applied and it is immersed in a water bath If there is a leak bubbles will develop The air bubbles that develop within a specific interval are evaluated by the worker tester Only gassing lids with a leak rate of lt 10 mbar l s are approved 6 1 1 Scope of delivery Jemen c
78. y effects by the ground material are not taken into account lt 79 FRITSCH A Be extremely careful if solvents are used 60 ml isopropanol in an 80 ml grinding bowl results in the development of the following pressure and temperature Temperature of grinding bowl Pressure in the grinding bowl wall C bar 50 1 73 2 86 5 109 8 124 10 5 132 13 139 14 148 19 149 20 The overpressure limit for fluororubber flat seals is reached at 120 C and for silicone seals at 149 C Here is an example of the pressure and temperature development during an actual grinding operation Grinding balls 120 g 0 4 0 7 mm ZrO Grinding bowl 80 ml ZrO Material to be ground 10 g aluminium oxide with feed size d 9 20 um Addition 30 ml water Speed 1100 rpm Time min Bowl 1 C Bowl 2 C 10 124 119 15 140 136 Other configurations or material to be ground may result in high temper atures being reached much sooner C Because the gases and solids are mixed completely in the grinding bowl pure gas is never discharged Material to be J ground is also discharged To clean the mills see amp Cleaning on page 104 30 FRITSCH u 5 1 3 Grinding bowl lid The grinding bowl lids seal the grinding bowl gastight after manual pre tensioning see also Safety measures against an excessively high pres sure on page 40 The locking hooks are designed to withstand an internal grinding bowl

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