Operating instructions PLANETARY MICRO MILL PULVERISETTE 7 premium line Valid starting with: 07.
Fritsch GmbH Milling and Sizing Industriestraße 8 D - 55743 Idar-Oberstein Telephone: +49 (0)6784/ 70-0 Fax: +49 (0)6784/ 70-11 email: info@fritsch.de Internet: www.fritsch.
Certifications and CE conformity Certifications and CE conformity Certification Fritsch GmbH has been certified by the TÜV-Zertifizierungsgemeinschaft e.V. An audit certified that Fritsch GmbH conforms to the requirements of the DIN EN ISO 9001:2008. CE Conformity The enclosed Conformity Declaration lists the guidelines the FRITSCH instrument conforms to, to be able to bear the CE mark.
Table of contents Table of contents 1 Safety information and use........................................................... 8 1.1 Requirements for the user..................................................... 8 1.2 Scope of application............................................................... 8 1.2.1 Operating principle............................................................. 9 1.2.2 Drive motor and speed regulation...................................... 9 1.3 Obligations of the operator..........
Table of contents 6 5.1.3 Grinding bowl lid............................................................... 5.2 Choice of grinding bowls and grinding balls........................ 5.2.1 Useful capacity of the grinding bowls............................... 5.2.2 Size of the grinding balls................................................... 5.2.3 Number of balls per grinding bowl (independent of the material quantity)............................................................. 5.2.
Table of contents 7 6.1.3 Hose adapter for grinding bowl gassing............................ 6.1.4 Removing the gassing lid in individual steps..................... 6.2 Gassing lid with stainless steel, swagelok hose couplings... 6.2.1 Scope of delivery / lid design............................................ 6.2.2 Fitting the gassing lid on the grinding bowl...................... 6.2.3 Hose adapter for grinding bowl gassing............................ 6.2.4 Removing the gassing lid in individual steps...
Table of contents 8 Cleaning...................................................................................... 8.1 Grinding elements.............................................................. 8.2 Mill..................................................................................... 8.2.1 Removing the grinding chamber cover........................... 9 Maintenance.............................................................................. 103 10 Guarantee terms..............................
Safety information and use 1 Safety information and use 1.1 Requirements for the user This operating manual is intended for persons assigned with operating and monitoring the Fritsch the 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.
Safety information and use 1.2.1 Operating principle a b c Rotation of the grinding bowl Centrifugal force Rotation of the support disc The source material is crushed and ground by grinding balls in a grinding 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.
Safety information and use Neither compliance with this manual nor the conditions and methods used during installation, operation, use and maintenance of the the PULVERISETTE 7 premium line can be monitored by Fritsch GmbH. Improper execution of the installation can result in property damage and thus endanger persons.
Safety information and use ENVIRONMENT! This symbol and keyword combination points out a possibly hazardous situation that can result in environmental damage if not avoided. Special safety information To call attention to specific hazards, the following symbols are used in the safety information: DANGER! This symbol and keyword combination points out a directly hazardous situation due to electrical current. Ignoring information with this designation will result in serious or fatal injury.
Safety information and use Safety information in the procedure instructions Safety information can refer to specific, individual procedure instructions. 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. Example: 1. Loosen screw. 2. CAUTION! Risk of entrapment at the lid. Close the lid carefully. 3. Tighten screw.
Safety information and use Do not remove the information and warning signs. Caution! Hot surface Caution! Crushing hazard 1.6 Device safety information n Only use genuine accessories and genuine spare parts. Failure to observe this instruction can compromise the safety of the machine. n Accident-proof conduct is to be strictly followed during all work.
Safety information and use 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 Ä Chapter 5.1 ‘Safety information’ on page 27 and Ä Chapter 5.8.2 ‘Safety measures against an excessively high pressure’ on page 40. – Never use brute force to open the grinding bowl.
Safety information and use CAUTION! – Wear hearing protection! Above a sound level of 90dB(A) – Wear safety gloves! The grinding bowls may get very hot. See Ä Chapter 1.8 ‘Hazardous points’ on page 16, Ä Chapter 5.8.1 ‘The effect of high temperature’ on page 39 and Ä Chapter 5.12.10 ‘Cooling the grinding bowl’ on page 58. – Do not grind with the device for several hours in succession without cooling phases. Risk of overheating! – The device may not be run without supervision.
Safety information and use n The grinding chamber cover must always be closed during grinding. n When the grinding chamber cover is open, the mill's mechanical unit is locked mechanically to prevent it from starting. 1.8 Hazardous points n Crushing hazard when opening and closing the grinding chamber cover (the closing force can be adjusted, consult Fritsch GmbH). n Crushing hazard when adjusting the control display. n Crushing hazard when using the locking lever.
Safety information and use 1.9 Electrical safety 1.9.1 General information n The main switch separates the device from the power supply with two poles. n Turn off the main switch if the planetary micro mill is "out of service" for prolonged periods (e.g. overnight). 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.
Technical data 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: n Wide range input 100-240 V ± 10 %.
Technical data 2.7 Electrical fuses n Fuses on the back of device: 2x10 A T 2.8 Material n Maximum feed amount in the case of hard material approx. 5 mm n Maximum feed amount 2 x 35 ml 2.9 Final fineness n Dry grinding up to d50 < 20 µm (depending on the material) n Wet grinding up to d50 < 0.
Installation 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.
Installation Grinding bowls made of tempered steel may have recesses on the surface caused during production. They do not have 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 n Set up the planetary micro mill indoors, on a flat and firm surface.
Installation 3.4 Ambient conditions WARNING! Mains voltage! – The device may only be operated indoors. – The surrounding air may not carry any electrically conductive dust. – Maximum relative humidity 80% for temperatures up to 31°C, linearly decreasing down to 50% relative humidity at 40°C. n The room temperature has to stay between 5 - 40°C. n Altitudes up to 2000 m n Degree of pollution 2 according to IEC 664. 3.
Installation 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 prevent operational transient emissions. The possible leakage currents resulting from filtering measures can trigger a conventional residual current circuit breaker in the mains line.
Initial start-up 4 Initial start-up Switch on the device only after all work as described in Ä Chapter 3 ‘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). 2. Gerät am Hauptschalter einschalten. 3. The display lights up. 1. Grinding station 1 is moved into the loading position. 2. The grinding chamber cover opens. 3. Check if grinding station 1 is empty (no bowl inserted). 4.
Initial start-up 9. You can make various settings in the next menu. Select the "Parameters" menu item. 10. A sub-menu appears in which you can enter the speed using the input keys. Set the speed to 100. 11. Press the "<" button to save your entry and return to the main menu. 12. Press the "Start" button to close the grinding chamber cover and start the safety check. 13. Various sensors check the bowls and the closing mechanism. That will take a few moments.
Initial start-up 14. The sensors detect that the grinding bowls are not present. 15. Press the ">" button to open the grinding chamber cover and grinding station 1 is moved into the loading position. 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.
Using the device 5 Using the device 5.1 Safety information 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.
Using the device NOTICE! The planetary drive is provided by the main disc via a toothed belt drive. Constant high loads stress the toothed belt severely, and may even damage it. High loads may be: heavy loads, high speeds, high temperatures, long operating 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.
Using the device 5.1.2 Overpressure relief of the grinding bowls The grinding bowl seals have a sealing effect but are also for overpressure 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.
Using the device 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 wall [°C] Pressure in the grinding bowl [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.
Using the device 5.1.3 Grinding bowl lid The grinding bowl lids seal the grinding bowl gastight after manual pretensioning (see also Ä Chapter 5.8.2 ‘Safety measures against an exces‐ sively high pressure’ on page 40). The locking hooks are designed to withstand an internal grinding bowl pressure of up to 40 bar.
Using the device 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 centrifugal forces during grinding may cause the grinding balls to penetrate the bowl's wall and damage the mill.
Using the device Exception: Tungsten carbide balls (<20 mm) may be temporarily (a few minutes) combined with grinding bowls made of tempered steel. 5.2.1 5.2.2 Useful capacity of the grinding bowls Grinding bowl 20 ml 45 ml 80 ml Useful capacity (material to be ground) 1-9 ml 3-20 ml 10-30 ml Size of the grinding balls Type of feed material Suitable ball diameter Hard samples with a maximum feed size of 5 mm 15 mm / 20 mm Average feed size of 0.5 – 1 mm 15 mm / 10 mm Fine material 0.
Using the device 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.
Using the device 5.2.
Using the device 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. 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.
Using the device CAUTION! Never operate the device without material to be ground, otherwise the grinding balls and grinding bowl will be damaged. 5.6 Factors with an impact on grinding 5.6.1 Running time (grinding duration) 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. 5.6.
Using the device 5.6.5 Weight of the balls (type of material) A higher mass (specific weight) of the grinding balls accelerates grinding. (see table in Ä Chapter 5.2 ‘Choice of grinding bowls and grinding balls’ on page 31). 5.7 Dry grinding Below a particle size of approx. 20 µm, the surface forces prevail and the material to be ground starts to "stick". Additional dry comminution can be achieved by adding surface-active substances to the material to be ground.
Using the device 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 particles 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".
Using the device 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 brute force to open the bowl 5.
Using the device 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. NOTICE! After releasing the pressure via the press-on sleeve, this and the valve plugs (6) must be cleaned thoroughly before further grinding processes. If this is not done, the tightness may be reduced due to residual sample material.
Using the device 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). 2. Push the locking hooks (4) inwards completely at the top end and place the lid (2) on the bowl (1). 3. The lid (2) is now lying on the small lug (a) of the locking hook (4) on the edge of the bowl. 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.
Using the device 5. Release the locking hooks (4) and push them together at the bottom end until they engage and are exactly vertical. 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. + 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.
Using the device 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? à remove any coarse dirt. 2. Is the grinding bowl adapter clean on the inside? à remove any coarse dirt. 3. Are the grinding bowls sealed correctly (see Ä Chapter 5 ‘Using the device’ on page 27). Inserting the grinding bowls 1. Open the clamping bracket (10). 2.
Using the device 5.9.5 4. Push the locking element (11) down on the bowl holder. à the grinding bowl is lowered within the mounting device. 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.
Using the device 2. Push the locking element (11) down on the bowl holder. 3. The grinding bowl is unlocked and moves up a few millimetres. 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.
Using the device 6. Push the clamping brackets (10) down until they engage in the bracket guides (12) provided and can not be moved down any further. 7. The loading position can only be changed if the locking elements (11) and clamping brackets (10) that are not in their initial positions and block the milling mechanism reach their initial positions again correctly.
Using the device 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. To what extent the heating up of the material to be ground needs to be observed naturally depends on the corre‐ sponding sample in each individual case.
Using the device If prolonged blow-off noises and the discharge of source material suspension 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. 5.12.1 Program sequence after switching on 1. Turn the device on at the main switch. 2.
Using the device 6. Grinding station 1 is moved into the loading position. The grinding chamber cover opens automatically. 7. Insert the grinding bowl (Ä Chapter 5.5 ‘Filling the grinding bowl’ on page 36), loaded with the sample (Ä Chapter 5.9 ‘Handling the grinding bowl’ on page 40) and closed correctly, in the grinding bowl holder (Ä Chapter 5.9.4 ‘Inserting the grinding bowl in the grinding bowl holder’ on page 44). 8. You can press the Close button (c) to close the grinding chamber. 9.
Using the device 13. Press the Start button à the grinding chamber is closed and the safety check starts. 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. 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.
Using the device 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. Depending on the choice of the ball size, 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.
Using the device 5.12.3 Overload If the planetary micro mill is overloaded, the speed is reduced. The reduced speed flashes on the display. 5.12.4 "Program" menu item Grinding cycles can be programmed, saved and selected here. 1. Press the "Menu" button in the main menu. 2. Then press the "Program" button ￫ A new window appears. 3. The "Current" column shows the current parameters of previous entries. 4. The "Program" column shows the data previously stored under button 1.
Using the device 5.12.5 5.12.6 Saving the current data 1. First select the program section that is free or to be overwritten. 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 displayed in the "Program" column. 1. Select one of the programs 1..8, the various parameter records are displayed in the Program column. 2. Press the "Load" button to transfer the program data record.
Using the device 5.12.7 3. Press the "<" button to return to the main menu. The program is disabled by manual input e.g. of the speed (see Ä Chapter 5.12.1 ‘Program sequence after switching on’ on page 49). 1. Select Menu. 2. Select Clock. 3. Select the time base for the internal clock.
Using the device 4. Press the "<" button to confirm your entry 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 "<" button to confirm your entries ð 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.
Using the device To tolerate this imbalance within specific limits, you can set the shutdown threshold. Touch the adjustment bar or move it back and forth by applying slight pressure. Press the "<" button to confirm your entries Small setting values make the measuring system more sen‐ sitive, and high values make it less sensitive. 5.12.9 Switching off 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.
Using the device 3. 5.12.10 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. 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.
Accessories 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 <10-4 [mbar l/s] are approved. 6.1.
Accessories 6.1.2 Fitting the gassing lid on the grinding bowl 1. Place the silicone flat seal (2) on the edge of the bowl insert. 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 (Ä Chapter 5.9.3 ‘Closing the grinding bowl’ on page 42).
Accessories 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. 6. Push the central handle (9) down by hand until the resistance increases.
Accessories 6.1.3 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. 8. This is what the closed grinding bowl looks like. Hose adapter for grinding bowl gassing 1. Push the locking lever (11) of the connection on the hose inwards.
Accessories 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. 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 turbulence in the grinding bowl or of the material to be ground when it is inserted. 4. 6.1.
Accessories (10) Actuating pin 2. Unscrew the two actuating pins (10) with a broad slotted screwdriver (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.
Accessories (5) Valve insert 5. Turn the two valve inserts out of the valves using 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.
Accessories 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 <10-4 [mbar l/s] are approved. 6.2.1 1 2 3 4 5 Scope of delivery / lid design Compl.
Accessories 11 Single head wrench, size 11 6.2.2 Fitting the gassing lid on the grinding bowl 1. Place the silicone flat seal (9) on the edge of the bowl insert. 2. Place the gassing lid insert (8) with the seal gassing valves (3 and 4) and actuating pins (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.
Accessories 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 (Ä Chapter 5.9.3 ‘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. 6. Push the central handle (1) down by hand until the resistance increases.
Accessories 6.2.3 a Hose adapter for grinding bowl gassing Quick-release coupling structure with screwed pipe fitting b Quick-release coupling connector with screwed pipe fitting 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.
Accessories 7 4 5 6 8 2. Unscrew the two actuating pins (7) with a broad slotted screwdriver (tightening torque approx. 4-5Nm = maximum manual force) 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. Remove the seals (5 and 6) from under the valves. The seals are deformed by the contact pressure.
Accessories 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 measurement. Grinding balls with a diameter of up to 0.8 mm or grinding balls with a diameter of 1.
Accessories 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: 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).
Accessories 5. Undo the two screws (D) of the battery compartment using a hexagon 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 certain amount of force.
Accessories 6.3.3 Configuration of transmitter ID and data transmission frequency The measuring/transmission unit (12) is equipped with four configuration switches for setting the transmitter ID and data transmission frequency. 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.
Accessories 6.3.3.2 Transmission frequency setting options Transmission every Switch 3 Switch 4 1 second OFF OFF ½ second ON OFF ¼ second OFF ON automatic ON ON 1-second transmission is the default value. For automatic transmission, the 1 / ½ / ¼ 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 battery's service life. 1-second operation results in the longest time span.
Accessories 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 guarantee 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.
Accessories 5. Switch on the transmitter with the On/Off button (A) and insert the bowl as described in Ä Chapter 5.9.4 ‘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, retighten them. 6.3.
Accessories 6.3.6 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 illustrated) 4. Close the rear panel of the housing again and screw it tight. Activating EASY GTM If the device is protected by SOP mode (Ä Chapter 7.1 ‘Standard Opera‐ tion Procedure’ on page 92), please contact the PULVERISETTE-7 administrator.
Accessories 1. Select Menu. 2. Select "EasyGTM" sub-menu. 3. Activate EASY GTM. 4. The inverted button indicates the current status.
Accessories 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! Depending on the setting of the operating mode, see Ä Chapter 6.3.9 ‘Selecting the operating mode’ on page 82, the device stops the grinding process and opens the grinding chamber cover or reduces the speed gradually until a minimum speed is reached in order to achieve an optimal cooling effect. 2.
Accessories 6.3.8 Entering the pressure limit 1. Select the maximum pressure input. If the max. pressure is reached, the device stops the grinding process and goes into cooling mode! Depending on the setting of the operating mode, see Ä Chapter 6.3.9 ‘Selecting the operating mode’ on page 82, the device stops the grinding process and opens the grinding chamber cover or reduces the speed gradually until a minimum speed is reached in order to achieve an optimal reduction of pressure. 2.
Accessories 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 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.
Accessories 6.3.11 3. Deactivate EASY GTM. 4. Press the[<] button to confirm your entry and return to the main menu. 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 thoroughly 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 necessary.
Accessories d socket head screws When inserting the locking ring (11), make sure that 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 running water as described in Ä Chapter 8.1 ‘Grinding elements’ on page 101. 6.3.11.
Accessories 6.3.12 Battery arrangement According to the "DIRECTIVE 2006/66/EC OF THE EUROPEAN PARLIAMENT AND COUNCIL as of 6th September 2006 on batteries and rechargeable batteries and on old batteries and old rechargeable batteries 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 legislation on the product responsibility for batteries and rechargeable batteries (BattG) as of 25.06.
Accessories 6.4.1 Design 1 2 3 4 5 6 7 6.4.2 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 Handling 1. Remove the bowl with the balls and the suspension from the device after grinding and remove the lid (Ä Chapter 5.9.2 ‘Opening the grinding bowl after a grinding operation’ on page 41).
Accessories 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 (Ä Chapter 5.9.3 ‘Closing the grinding bowl’ on page 42). 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 emptying device. 6. Inject the air in the syringe (1) into the bowl.
Accessories 6.4.3 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 procedure 5 to 10 times. 12.
Accessories 2 3 4 5 6 7 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 6.5 Compl. counterweight 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.
Accessories 6.5.2 Handling 1 2 3 4 5 6 Lock nut Rubber washer Compensating washers, 25 g each Counterweight 2-hole face wrench Pipe wrench 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 of the completely filled grinding bowl. (+/-12.5 g) 3.
Accessories 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-tightened. 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.
General and optional settings 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.
General and optional settings 7.1.1 Activating SOP mode 1. Enter a number between 1 and 9999; 2. Then "Save" it; 3. Press the "<" button to return to the main menu. ð 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 "<" button to return to the main menu. If the device is switched off, SOP mode is active again.
General and optional settings 7.1.3 Deleting SOP mode 1. Deactivate the mode (Ä Chapter 7.1.2 ‘Deactivating SOP mode’ on page 93) 2. Enter pin code 0000 and "Save" it 3. Press the "<" button to return to the main menu.
General and optional settings 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.
General and optional settings 7.3 Language change After selecting the national language, all other texts are displayed in the selected language. Press the "<" button to confirm your entry and return to the main menu.
General and optional settings 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 "<" button to save your entry and return to the main menu.
General and optional settings 7.5 Information The "INFO" button can be pressed to access system information. The n operating hours, n the firmware version and n the bowl materials are displayed here (if they were detected during a START procedure). n Press the "<" button to return to the main menu.
General and optional settings 7.6 Interfaces In the standard case, the device is equipped with a USB port. 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 "<" button to save your entry and return to the main menu. 7.7 Firmware update 1. Switch off the device. 2.
General and optional settings 3. Connect the USB cable and only then switch on the device. The USB port is now automatically activated. 4. Start the 'PROGRAMMER.EXE' software and then select the firmware file for programming. 5. Select the newly installed COM port here 6. Press 'Program' to start the update. 7. After programming 8. Now, connect the flasher software. 9. Switch off the planetary micro mill (not the computer!) for a few seconds. 10.
Cleaning 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.
Cleaning 8.2.1 Removing the grinding chamber cover 1. Remove the 4 screws from the side of the housing using a screwdriver. 2. Then, carefully tilt the grinding chamber cover to the right. 3. 3 connectors now need to be released. 4. After doing this, the cover can be lifted off completely and the grinding chamber can be cleaned. 5. To fit the grinding chamber cover, proceed in the reverse order. DANGER! Do not allow any liquids to flow into the device.
Maintenance 9 Maintenance DANGER! Mains voltage! – Maintenance work may only be performed by specialised personnel. – Before beginning with maintenance work, unplug the mains plug and protect the device against being unintentionally switched back on. – Put safety equipment back into operation after maintenance work. – Indicate maintenance work with warning signs. We recommend keeping a safety logbook Ä Chapter 12 ‘Safety logbook’ on page 108, where all work (maintenance, repairs......
Guarantee terms 10 Guarantee terms Guarantee period As manufacturer, FRITSCH GmbH provides – above and beyond any guarantee 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 discretion.
Guarantee terms Costs not covered by the guarantee This guarantee excludes 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 guarantee.
Exclusion of liability 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 maintenance.
Exclusion of liability Fritsch GmbH excludes any liability, warranty, or other obligation to compensate for damages, regardless of whether this liability, warranty, or other obligation is explicit or implicit, contractual or arising from unlawful acts or prescribed contractually, by law, or otherwise.
Safety logbook 12 Date Safety logbook Maintenance / Repair Name - 108 - Signature
Index 13 Index A F Accident prevention . . . . . . . . . . . . . . . . . . . . . . . . 8 Activating EASY GTM . . . . . . . . . . . . . . . . . . . . . . 78 Activating SOP mode . . . . . . . . . . . . . . . . . . . . . . 93 Adjustment options of the transmitter detection . . . 74 Ambient conditions . . . . . . . . . . . . . . . . . . . . . . . 22 Authorised persons . . . . . . . . . . . . . . . . . . . . . . . . 8 Filling quantities of grinding bowls . . . . . . . . . . . . Filling the grinding bowl .
Index Selecting the grinding balls . . . . . . . . . . . . . . . . . . 31 Selecting the grinding bowl . . . . . . . . . . . . . . . . . . 31 Selecting the operating mode for Easy GTM . . . . . . 82 Set-up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21 Setting the time control . . . . . . . . . . . . . . . . . . . . 55 Size of the grinding balls . . . . . . . . . . . . . . . . . . . . 33 Skilled workers . . . . . . . . . . . . . . . . . . . . . . . . . . .
© 2012 Fritsch GmbH Milling and Sizing Industriestraße 8 D - 55743 Idar-Oberstein Telephone: +49 (0)6784/ 70-0 Fax: +49 (0)6784/ 70-11 email: info@fritsch.de Internet: www.fritsch.
